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IngInzano
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| Joined: 21 Apr 2005 |
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| Location: Uruapan Michoacan Mexico |
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How to extract Psudoephedrine sulfate from mixture.....
Wed Apr 27, 2005 10:54 am |
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Hi all
alguien sabe un metod for extraction of pseudoephedrine sulphate to pills, and pseudoephedrine sulphate ------> HCl -pseudoephedrine ?
Tanks .
Alguien Habla Espaņol aqui ?
Saludos desde Mexico   |
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java
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| Joined: 07 Feb 2005 |
| Posts: 736 |
| Location: The Mexican Republic |
21796.14 Points
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Saludos
Wed Apr 27, 2005 8:30 pm |
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Saludos,
No puedes hacer lo que quieres hacer con ephedrine sulfate? Convierte el sulfate a la base the ephedrine el cual es un aceite, en el sentido de que se puede separar de el sulfato y despues puedes hacer lo que quieras con esa base. Lo que tu quieres saber es como sacar la ephedrina en forma de sal de sulfato y convertirla a ephedrina hidrochloride......pero no es necessario si vas hacer algo mas alla de la ephedrina hidrochloride.
Estas tratando de hacer, el cual no les gusta que se mencione, lo llamaremos methedrine. Sabes como trabajar empezando con la base? ya sea de ephedrina o de pseudoephedrina.....? Porque no te vas y visita WD, o sea wetdreams donde se platica en la tercera persona "alguien que conoci"=AQC, y se presta mas a esta clase de quimica, porque aqui hay poco de eso y mas de metodos hacia lo mismo pero empesando con otros quimicos .
Tambien soy miembro en ese lugar. Pero si quieres seguir con el projecto de "alguien que conoci"=AQC, entonces lo haremos......bienvenido,....java (tambien en Mexico)
Nota:
Recuerda cuando quieras decir "yo" usa AQC en tu commentario..... |
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IngInzano
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| Joined: 21 Apr 2005 |
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| Location: Uruapan Michoacan Mexico |
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:) Desde la Huacana :P
Wed Apr 27, 2005 11:47 pm |
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Me alegra encontrar alguien que hable el idioma de Cervantes, Fijate que AQC, quiere hacer un poco de "vidrio" cristal pues  , Este conocido, solo sabe trabajar El clorohidrato de pseudoEfedrina, entonces, quiere aprender a extraer ya sea la base libre, de las pastillas de afrinex, que vienen en forma de sulfato, y saber de un metodo para hacer lo mencionado, antes, osea ... el problema es que quiere trabajar con afrinex, osea con sulfato de Ephe, pero no sabe ni extraer el sulfato en sal o cristales , ni tampoco extraer de las pastillas la base libre, teniendo el Clorohidrato, se sabe bien llegar al Cristal, pero pos el sulfato es algo totalmente nuevo esa persona que conoci
Gracias por el comentario JAva.
Saludos desde la Sierras Michoacanas |
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java
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Informacion sobre como sacar .......
Thu Apr 28, 2005 6:19 pm |
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Estoy buscando en los archivos la informacion para que AQC pueda lavar y sacar la sal de sulfato , entonces hacerla base y si tanto quiere el hidrochoro , el metodo de hacer la base sal de hidrochloro, pero ten paciencia usa la funcion the mensajes PM si tienes preguntas, el cual cada miembro tiene. Nadien te escribe con su propio e-mail por causa de seguridad,.......java
Last edited by java on Thu Apr 28, 2005 10:38 pm; edited 1 time in total |
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java
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java
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Thu Apr 28, 2005 10:49 pm |
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Esto se encontro en WD tiene informacion sobre el sisntesis empezando con la base......java
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| Quote: |
Originally posted by fishinabottle
[br]Thats a lot, but well worth reading!
from the-hive:
| Quote: |
.........
First, I feel I must dispute some stuff that has been layed down here - in the WizardX write-up. In this write-up the author bases most of his work on calculations of the necessary ratios of HI to E and HI to I2. He gives an equation that goes like this: P + 3I2 + 3H2O __> H3PO3 + 3HI. From this equation, he then states that, therefore, The ratio of HI to I2 is 3:3 (1:1).
This equation is, IMHO, not balanced and incorrect because it fails to account for the missing 3 atoms of Iodine. 3I2 represents 6 Iodine atoms, since they travel in pairs. So, the correct equation should have been this: 2P + 3I2 + 6H2O __> 6HI + 2H3PO3. So now, what we really have in the flask is 6.6 or so molar equivalents (atoms) of Iodine per mole of ephedrine, as the HCl salt. Normally, then, I'd be thinking, "well, OK- there's twice as much Iodine in this reaction as the decription would lead us to believe. Up to a point, an excess of Iodine just helps the reaction along, everything else being the same... but then the real problem surfaces. If one looks at the amount of water or acetic acid being employed in the examples given and does a quick calculation to illustrate what the resulting solution's strength, in terms of %wt/wt of HI contained in the solution once HI has been formed in-situ, we see that around 34g HI added to 150ml h2O combine to make an aq. sol'n that is approx. 18%HI. This is a fairly weak HI sol'n if we can agree that high concentrations of HI in the reaction medium favor a decrease in reduction time. I'm guessing here, but I think it likely that decreasing solution concentration lengthens reaction time according to the inverse square law, which would mean that decreasing sol'n conc. by half would increase rxn time by a multiplier of 4, or thereabouts. In view of this, I feel it is incorrect to explain his result only in terms of his I2 to E ratios, while disregarding completely the volumetric concentration of the working reagent. It is precisely this that I feel is calling the shots in the reaction environment; not completely alone, mind you, but the major player, IMO. At least he didn't use an actual 3.3 mol. eq. in the rxn with so much solvent, because the next important consideration would have a further diluting effect: the 1st molecular equivalent of HI, in this reaction gets more or less 'taken out of the game' when HI (the stronger acid) displaces HCl (the weaker one) on the Ephedrine molecule, which results in the formation of Ephedrine Hydoiodide. Said ephedrine remains in that form until the reaction has been basified for work-up and so this ties up 1 whole equivalent of Iodine for the duration. This is probably OK if the reaction is jammed to the gills with HI to begin with, but such is not the case here. OK, enough about what somebody else said or did. I simply said all that so the following would not be confusing due to whats been said before. With all of that stuff in mind, let's now look at what I call the 'Classic' HI/RP reduction model. To me, this means the first version that was put forward publicly, to be applied to ephedrine. This was an adaptation of similar, earlier, HI/P reductions; some of which involved reducing benzylic -OH to -H, like the reduction of benzyl alcohol to toluene and also the reduction of a benzylic alcohol (mandellic acid) considered to be more easily reduced due to the presence of -COOH right next door. True to expectations, the 1st example was readily reduced in 57% HI with a minor amount of P, to keep the dog chasing its tail, and the later example was so easy to reduce that only approx. catalytic amounts of I2 were required to achieve rapid reduction. More detail than that escapes me; I'm going on recollection here.
The actual innovation involved here was the use of this reduction system on a substrate possessing an amine group adjascent to the hydroxyl bearing carbon. Understandably, the initial method employed merely utilized the commercially available 57% Hydriodic acid solution commonly used in labs for methoxyl determinations. Since it seemed to work well enough, albeit with somewhat long reaction times being required, compared to the 'usually encountered' HI/P reductions, there seemed little reason to fix what wasn't broken. Of course, the rxn evolved in the direction it has because of all the pressure the Feds have put on chems via their precursor control program and just being the rag pickers we all know they are. Trouble is, since there was never an 'applicable' reaction history for this method, as applied to this type of substrate, underground chemists were looking at a pretty blank slate, as far as deriving an optimization strategy by extrapolation from previous lines of the developement of this reduction. So, developement proceeded along a few different lines, each representing what that operator felt would best favor the mechanism he (or she) felt was the center of the reaction. Of all the different strategies I've examined and all the various rationales I've listened to that purport to support these strategies, only those advanced by Worlock seem to me to fit the model I perceive as being valid. I may not entirely agree with ALL his conclusions and I also may differ some about just how informative some of his visual cues are, in the practical sense, unless one stays strictly within the exact method he describes. That said, I'd like to explain what I feel is the key to optimizing this reduction system within the definitions I've already set out. I believe that what is paramount is that the volumetric solution concentration of HI in the reaction environment be kept as high as possible during the last, rate limiting, step, up to the point at which there is significantly too high a ratio of HI to available solvent for the HI to remain bound in the solvent at the temp of the rxn. This kind of "fuming" HI solution is rather like fuming H2SO4, in that it promotes dehydration to an excessive degree, IMHO. Dehydration conditions at this stage of the game, I feel, only serve to favor side reactions like the formation of unwanted aziridines via ring closure, which lead to further hydroxylic cleavage of this compound to form phenylacetone as well as other similar side routes that lead to naphthalene compounds by way of coupling : the Wurtz and similar paths. All of these 'dirt road' type of side reactions are aided by increasing heat under conditions of high enough acidic concentration to bring about elimination/dehydration between carbon and oxygen and also between carbon and nitrogen, at the adjascent carbon. Now that I've drawn a map to where I believe one should go, lets examine how best to arrive there in good fashion. For this, I like to focus completely on the 'reaction environment'. In a best case scenario, it would be just peachy if one could set it up so that a constant, unchanging solution concentration of either right at or just below 57% HI could be maintained for the duration of phase 2, at least, so as to provide optimum conditions for the rapid reduction of Iodoephedrine Hydroiodide to ---- Hydroiodide. Looking at it one way, we could say that we need 1 mol. eq. of Iodine to be used to form the HI salt of the substrate and another to replace -OH at the benzylic position, plus - an additional amount sufficient (when ccombined with the correct amount of H2O) to provide a quantity of 57% HI that will suffice to act as solvent for the reaction itself. Of course, this is a simplified model in need of refinement. First, reality dictates that the process of reducing Benzylic -I to benzylic -H doesn't wait until the entire halogenation has run to completion. What will really happen is that there will be an equillibrium reached between Bz-I and Bz-H that changes from predominately Bz-I, at first, to Bz-H being the predominating species as the reduction nears end point. As one can readily see, this causes an increase in the abundance of available Iodine in the reduction media as rxn progesses, causing a concommitant increase in sol'n concentration of HI. A separate event is occurring along side the increasing abundance of HI that accomplishes the same thing from the other side of the coin, so to speak. That is, as HI is being generated from the recycling I
2, available H2O is being depleted to satisfy the requirement for water during the transformation of P __>PI3 __> H3PO3. Of course, removing water causes the remaining (reduced) solution volume to become higher in HI concentration as a result. Since it seems that several separate processes can act concurrently to solidly bring about a sharp increase in HI concentration as rxn progresses, it appears that proper steps taken to blunt that rise should ease some of the possibly unnecessary violence, smoking, etc. that can jeopardize success near the end of a water starved or ' Push-Pull' type reaction, hopefully without sacrificing yield or going too far and causing it to slow so much that undue reflx time will be required to finish the job. One of the things I see 'being' done in this vein is (in a P/P) to reduce the Iodine used to about 1:1 with E weight. This variant, since the first mol. eq. of Iodine is tied up forming the HI salt of E,leaves only about 1/2 mol. eq. of Iodine left to add to the carbocation at the benzylic position (halogenation) and also be available to provide enough free HI to fuel the reduction itself. This is elegant; its like 'leaning up' the fuel mix in a carburetor to increase economy and combustion efficiency without sacrificing horsepower. That's Worlock for you!! Typical simple but insightful move to slay two dragons with but one thrust of the sword... In writings by that same author, we will see that an amount of water roughly equal to 3ml per oz of E used in the rxn is added to the mix early on. After subtracting for Iodine bound to E as the HI salt, we can see that this ends up giving us about 1ml of water for every 3.5 grams of 'available' Iodine. If we assume that, say half of the available Iodine, at any give time, is busy forming the halocarbon (C-I) linkage and the other half is providing available 'free' Iodine for the reduction (via dissociation) then it should surprize no one that 1ml of water combined with 1.7grams of Iodine yields a solution of approx. 50something% concentration in the reaction environment. While the consumption of water still wants to cause an increase in sol'n concentration by its leaving, the concurrent creation of H3PO3 eases this somewhat by supplying this as an alternate solvent (its liq. at these temps), thus increasing dilution. Additionally, part of the water requirement is met via the -OH group departing the benzylic carbon. My personal preferrence is to use approximately 6 ml of water per oz of Iodine used (ex: 1g E:HCl/1.5g Iodine/.3 to.4g RP/0.2ml H2O). One half of the water is added at the start of the process and the rest added during the start of 'phase 2'. 'Phase 2', in my variant, consists of simply slowly raising the temp of the reaction to maintain a gentle reflux over a 3 to 4 hr period, although even less is actually required to complete the reduction. Similar factors influence the 'actual' amount of water that is optimal; how dry were the reagents as used, etc., but only slight adjustments are needed, on the order of plus or minus 10 to 15% to correct. To me, this system is much more forgiving without really sacrificing yield, although the reaction doesn't give the operator nearly as much 'feedback' to let him know how it is progressing. Experience with this reaction, however, does leave you with the ability to recognize signs of a slightly more subtle nature that one learns on his own very quickly, and in no time he can simply 'tell' when its done.
There is more that can be done, in my opinion, to optimize this reaction. Some of these things Swix has done (most, actually) at different times but, much as he hates to admit it, never has he undertaken to incorporate these variations all in a single reduction. They should still, however, be mentioned. The first one is to incorporate the base form of Ephedrine into this process, rather than the HCl salt. Why? Well, since the HCl is displaced by HI early on in the reaction, you could say - 'its gotta go anyway..... so why not? By itself that aint enough for me. However,I'm questioning what good is accomplished having that free HCl running around in the reaction mix. Cant see any, off hand....anyone else? I can see its potential to have a negative effect on the reduction, though, because it adds to the acidity of a solution that needs no extra push there (quite the opposite) and it also most likely competes with Iodine during halogenation. While that competition is pretty nuch tilted in favor of Iodine, for those few times when Chlorine might 'win the toss' it then causes a bit more grief in the reduction its not nearly as good a 'leaving group' as Iodine, and so requires a fair bit more energy to pry it off that carbon. Now, I heard Worlock's ccomments earlier vis-a-vis the character of the Nitrogen when in the base form being such that it causes an overly vigorous reaction with the RP, etc. Does he mean to refer to the analagous rxn between Iodine and Ammonia to finally form Nitrogen Triiodide? Or, does he mean simply salt formation via dissociation? I dont yet have a solid opinion as to just how this idea fits in to the overview, but in any event, the free base of ephedrine can be employed in such a fashion, I believe, as to preclude this being a tangible problem, in the following way: At the start, the flask is charged with a minor amount of RP (1/4 of total), half of the water and 1 equivalent of Iodine. The Ephedrine Base is then added to the cooled pre-formed HI sol'n and kept cool until it all has had a chance to form the HI salt (shortly). At this point, you should be dealing with no free base E and the remainder of the reduction should proceed without the aformentioned effect and without a bunch of free HCl running around & getting in the way of our Iodine. If one always harvests one's Iodine from the reaction liquid after basification and NP extraction to remove the product, this gives your Iodine back to you free of Chlorine contamination. That's a plus. Another modification that I favor strongly is the use of a mixed Phosphorus system. By that, I mean; the use of Hypophosphorus acid in 50% strength, along with a correspondingly decreased amount of RP added. Swix applied this concept only a couple of times, but liked the way it ran. The first time, it was only done because it was decided to use the E as the free base. Swix added about 15ml of Hypo, as calculated to produce enough free HI to form the HI salt of the 50g of E base he'd planned to use. It just happens that this also left Swix with just about the exact amount of water he would have added at the first of the reaction anyhow. The salt was immediately formed without undue heat and after minimal cooling, the RP was added (75% of usual), followed by Iodine and, later on, the remaining water needed was just sufficient to initiate reflux moments after the application of gentle heat (hair dryer), with reflux continuing at a very moderate rate for approximately 45min to an hour. It was next heated on a hot plate (low setting,then between low & med) and began another sub bp reflux that required only minor heat input to sustain for about 1-1&1/2 hrs more. The yield was a bit over 80% on that and it pretty much jumped out of the pot clean. Lastly, I believe that glacial acetic acid could be employed, using only the water actually necessary to digest the P, etc, with some benefit attributable to solvent effects. This last notion is more purely speculative, as there is nothing really solid, IMO, to support a significant benefit derived from utilizing acetic acid in this type of system. It may only provide real help in more dilute reduction variants, but it should be experimentally determined, rather than dismissed. It may also be true that Acetic acid may be able to substitute for water, i.e., perform in analagous fashion to water in a reaction with P to cause Iodine regeneration. There may be some advantage seen there, if that proves to be true.
In a 1 Liter filter flask fitted with a tygon tube at the vac nipple is placed 30 grams of RP and 10ml of dist. water, followed by 15 g of Iodine. contents of flask are repeatedly swirled to mix well and time is allowed for the initial Iodine to react and more or less clear up before adding 20 grams of E base and mixing well. After cooling briefly, the flask is again charged with another 15 grams of Iodine, allowed to digest as before, and another 20 grams of E base added as before. This is repeated until 85 grams of E base has been added and about 65 grams Iodine has been added, any excesses of reagents being included in the last addition. Once done, the flask is cooled in an ice bath or similar contraption and the remaining 85 grams of Iodine is added in small (5 - 8g) portions with mixing. During the first few additions there will be a noticable warming of the flask and some bubbling may be observed. When this happens (or even if only warming is observed) the remaining 10 ml of dist. water is added with swirling and the top of the flask is immediately capped off with a rubber stopper. The tygon tube may be run to the outdoors or to a suitable fume trap. No reflux condenser will be required. Any further additions of Iodine required to add the entire 150 total grams will be done by adding the portions and recapping between additions, taking care to keep reaction moderated by advancing or retarding the rate of addition of the Iodine. Soon all the I is added and the Flask can be gently heated just enough to stimulate reflux. If it doesn't initiate on its own, dont be concerned, simply supply enough moderate heat to maintain reflux for a period of 3 to 4 hrs max.then proceed to last step. If reflux kicks on its own, thats all the better- maybe even get a slightly higher yield in some cases. Let it do its thing, in this case, only supplying heat as needed to keep it gently boiling for 2 1/2 to 3 1/2 hrs in order to drive it to completion. Smaller reactions can usually be conducted in slightly less time, but it doesn't hurt anything to give that extra time to max your return. Work up of the reaction liquid to recover product is the same as shown many times in other work. Recrystalization slowly from a hot concentrated alcoholic solution of the cleaned product gives a superior end result, IMHO. However, if one desires Really big xtals in the form of huge transparent shards, there is one other technique. To do this, one needs a goodly amount of cleaned product, because, like goldfish, the size of the container has a limiting effect upon the maximum size they can grow. This method grows them large enough so that that is the limiting factor. Start with nicely cleaned product and place it in a beaker just big enough to contain all the product, when compacted by hand. There should be a stir bar used for this in conjunction with a good magnetic stirring hot plate. From a separate beaker containing near boiling dist. water, add water in small amounts to the product. Your goal, here, is to get just enough water in the beaker with the product to barely dissolve it at close to the boiling point. Once that has been done, Place a thermometer well into the thick liquid and turn up the heat, while stirring at a moderate rate. Product will go into solution soon enough. Continue to heat and bring solution to a boil. You want to make sure the product is clean enough so that there are no solids floating around in the liquid (a tiny or very minor amount wont hurt, but too much may cause premature formation of crystals; smaller ones that we want here) and then watch the temp rise in the thermometer as it boils. Stop the heat and stirring as soon as the temp reaches 118 to 119?C. Once this happens, quickly but carefully transfer the beaker to a well insulated container and seal the top with a latex glove (or similar) to negate vapor loss. Place this insulated beaker inside of a well insulated and constructed ice chest and let stand undisturbed for at least 16 to 24 hrs, then remove and place in the fridge to cool. Once cool, the minor amount of water remaining in the beaker is removed by quickly subjecting the entire mass to vac. filtration, prefferably using a fritted disc type filter funnel, if you have one. Dont even try gravity filtration. In the time it takes, significant loss of initial crop will be incurred as water looses its cool and becomes a better solvent for the crystals.... As soon as the crop is filtered, the flask is changed so that the filtrate in it can be either recycled into the next xtal batch or evaped to grow a smaller crop, and the semi dry xtals on the funnel are immediately washed with a liberal amount of very cold acetone, pure at first, then with 33 to 50% ether (if you have it) added to the acetone. The resulting crop of crystals are beautiful to behold and, when conducted in 2 liter beakers or coffee pots with appropriately slow cooling, appear as huge masses of interlocked shards, some as long and thick as your forefinger. Some are nearly clear enough to read the Sunday paper through. The largest actually accomplished by Swix was a single mass of xtal shards, locked together and closely resembling a mass of display quality quartz xtals that weighed in at just under 380grams dry. Some bastard came up with enough $$$ to pry it out of Swix's fingers. Well do I get the award for longest post? This took me quite awhile to do, so I really hope someone found it worth reading, especially if some part of it sparks an idea that benefits someone who has need. For what its worth, it is my gift to you all.
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.......
Before I forget - about that 380g xtal.... "about the size of a football?... Not quite, really. Swix's fond recollection of this one (in a way, Swix sees them as his progeny)
does seems to make its image loom larger in his thoughts with the passage of time, but -no. In reality this one was born in a $0.50 thrift store coffee pot that impressed Swix with it's so desirable 1:1 dia. to height ratio, as this is often reported superior for birthing xtals. The density resulting from the xtal generation/regeneration growth cycle conducted in H2O in that way is about max obtainable, I beelieve. BTW, Swix discovered ths method of using water accidentally, about 7 years ago. Swix was, at that time sufferring from delusions of grandeur; thinking he was going to build big castles in the sky, be the "big dog" and get rich.... World domination was in the air. Big, ambitious plans were launched and big ambitious partners were brought together to carry them out. For a time everything seemed almost perfect. Swix got to do some thing he'd always hoped & dreamed; like having 3 50 liter set-ups in a row, permanently mounted to lattice support frames that are fixed to rollable reaction benches, etc.,etc. The work involved cant be imagined until you try it yourself, IMO. Swim was working under the basic premis " I'll sleep when I die..." and never actually left the 'farm' for entire 4 or 5 month stretches. That kind of shit will rattle a fella and so one time when Swim was boiling off the acid/H2O extract from a 22 liter HI/P run of about 10lb size. To avoid too much loss, heat is best moderated. All product was contained in 4 2liter (big) coffee pots being gently evap'd on two 12"X12" hot plates. Sleep was insistantly knocking on Swix's brain, so he decided he'd better shut down rather than risk that much loss by nodding off at the wrong time. Swix knows the value of always taking accurate notes and he correctly noted the temperature reached prior to shutting the heat, down on each pot. Not knowing how long sleep might claim him, Swim placed the still hot coffee pots full of product/water in a small, styrofoam, ice chest, wrapped in heavy towels and sealed with latex gloves. This container was then taped securely, labeled and placed in one of those thermo-electric coolers that was unused. More than 24 hrs of sleep was then gotten. By the time Swim was all rested up and ready to begin another marathon run, the 'soup' had been sitting at least 36hrs. 2 of the pots had only risen to 112 degrees C. These were clear with a slight yellow tint and denser than water by quite a bit. However, the ones that made it up to 117.5 and 119 degrees C were now a solid mass of stunning shards that looked like Godzilla versions of the ones Swim had always via slowly cooled or slowly evap'd conc. alcoholic mother liquors. At first it made NO sense to Swim, who had applied huge effort over several years: always seeking to avoid having moist product. As a solvent ideal for xtal growth, water was ruled out, along with water rich solvent systems, because it was 'assumed' that water would only allow the cooled/cooling solution to retain more product, hampering growth. Any solvent that holds more than its own weight of solute at room temp just seems a poor choice. Swix was wrong in this case and happy as a maggot in a cube steak to be wrong!!
Another thing that Swix has got wrong is contained within that last post. I reported in detail, from an historical
perspective, about the 'evolution' of the HI/RP RXN cuz Swix was there to see it first hand. However, the statement that was made regarding underground operators not having a reaction history in the literature that shows the reaction being carried out upon benzylic -OH with an amine function on the neihboring carbon was wrong. Swim still believes that any active operators were unaware of any examples existing in the literature back then. However, those poor sods didn't have a secret weapon like Polythene Sam in their midst. Data trembles in the presence of Polythene Sam and it is said that no fact is safe from discovery. One of Polythene's recent posts includes a link to his patent finder, which takes us right to the place that little factiod had been secreted. Well, anyhow - as you know, I could go on & on here but it is best I just end this with an idea. Possibly a carefully thought out series of identified variants of the IorHI/P-orH3PO2 rxn system could be described with specific method to be used and rxn size, etc. These 'experiments could be posted and then any bee that wants too can tackle part of the job of mapping out this system. Seems there's lots of bees interested in one or another variant, so every proposed variant should find a cross section of interested folks willing to investigate.
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No actual information was cut out, only some socialising at the beginning of the posts.
[:-goldfish]
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IngInzano
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Gracias por tu Ayuda Java
Thu Apr 28, 2005 11:05 pm |
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Gracias, me pondre a estudiar esos enlaces, de nuevo muchas gracias, por tus respuestas y tu atencion.
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ApprenticeCook
DILLIGAF
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IngInzano
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2.42 Points
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ESpaņol , Spanish :)
Sun May 01, 2005 3:02 am |
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| Esto esta Escrito en Espaņol, this Write in Spanish |
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QuickFitAbuser
Quality Control
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490.04 Points
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re: How to extract Psudoephedrine sulfate from mixture.....
Thu May 12, 2005 4:31 pm |
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Would have liked to see what this thread was all about.
Spanish?
Nice Quote/info, musta missed this earlier. |
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Sandmeyer
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203.32 Points
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Re: re: How to extract Psudoephedrine sulfate from mixture.
Thu May 12, 2005 5:00 pm |
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| QuickFitAbuser wrote: |
Would have liked to see what this thread was all about.
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it really can't be more unambiguous, as you can see, you really need a considerable amount of m3thamphetamine in your system in order to write 5000 words about something that can be said in couple of lines. |
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hAzzBEEn
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| Joined: 09 May 2005 |
| Posts: 126 |
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4955.86 Points
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re: How to extract Psudoephedrine sulfate from mixture.....
Thu May 12, 2005 6:08 pm |
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SWIM also wanted to try extracting Pseudo Base from sulfate pills (blue ones) with Loratadine. SWIM did some research and found very little. SWIM does think that posts 468062 & 333934 from the hive would help as I indicated in this post:
https://synthetikal.com/synthforum/about571.html
Sorry, you may have answered this question, but my Spanish is very rough. I read this entire post and followed the the link posted by Java, but none of the links from that page were working. Will any A/B extraction work?
Also I read, "but a jap/tetra wash, and then a/b will work", from this link:
http://12.162.180.114:90/synthetika/hiveboard/crystal/000499993.html
but I'm not familiar with this, and the hive posts that explain this in more detail aren't available (the ones I listed above). |
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loki
guinea pig
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| Joined: 09 Mar 2005 |
| Posts: 391 |
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14167.88 Points
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re: How to extract Psudoephedrine sulfate from mixture.....
Fri May 13, 2005 5:35 am |
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i dunno about the particular sulphate pills you are talking about, but then maybe i do
the ones i am referring to are named after a synonym of loratadine and a shortend word related to 'nasal', in a two-dose repeating release formulation intended to produce a 12 hour effect.
swim struggled with them three times playing with ethanol extraction and being ground up, but then out of the blue swim tried something different and they came out much cleaner and ... well it actually worked, nice crunchy pfed.hcl, a yield in the vicinity of 80%
these pills were that type with the second inner pill inside them, and the problem that was occurring in previous attempts was that nasty coating, a yellow plasticy substance. but the yellow goop is not even intended to dissolve anyway.
swim just took the pills, put them in distilled water in the microwave and nuked them for a minute or two, and in the process, the pills swelled up like baloons and the inner pill burst, dumping its contents into the water. having seen this lovely swelling process occurring, swim thought 'hmmm maybe this has successfully got the goods out without dissolving that gak'
so the liquid was filtered clear of the swelled burst inner pills and then an acid/base extraction was performed on the filtered liquid and the result was the aforementioned 80% yield of the most lovely pseudoephedrine crystals swim had ever seen. slightly contaminated with something unidentifiable (and yellow) but the result was clean enough to be successufully reduced in a phosphorus/iodine dehydration reaction
hope this helps somehow |
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java
Consumer
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| Joined: 07 Feb 2005 |
| Posts: 736 |
| Location: The Mexican Republic |
21796.14 Points
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re: How to extract Psudoephedrine sulfate from mixture.....
Fri May 13, 2005 8:03 am |
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Not to be left out of the spanish conversation, as I was trying to fill the need for a spanish speaking member. Basically he has a problem removing the ephedrine sulfate from some pills which contain an antihistamine. The problem is that the basic A/B is not practiced and so I recommended Mad Max's A/B.
The information provided deals with the solubility of ephedrine sulfate in water , hence I recommended the use of a solvent where the antihistamine isn't soluble.....homework.
Loki, good experimenting I will relate your findings to the member ........java |
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loki
guinea pig
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| Joined: 09 Mar 2005 |
| Posts: 391 |
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14167.88 Points
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re: How to extract Psudoephedrine sulfate from mixture.....
Mon May 16, 2005 12:41 am |
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I was originally going to put this post on this thread but since it turned into a monster I thought it should probably go by itself. The post I wrote can be found here:
https://www.synthetikal.com/synthforum/viewtopic.php?p=4875#
Unfortunately I don't know spanish either, but the process of thinking about it as related to the tablets I know about, at a certain point in the process the creative thought kinda took on a life of its own. I spent a bloody long time trying to make sure that it was decently structured and had no spelling or grammar errors, but I'm sure that I'll spot more now that I've committed it to the public eye.
Anyway, the post is, in the first part, about a method virtually guaranteed to work, as most of its methods are already tested, the second part is a kinda half-though out method which is a possibility, but the third part is the part which I am most excited about, which involves a method which possibly could be virtually universally applicable because it starts with deliberately making everything insoluble via salt saturation, acidifying fatty acids to separate them, and forming a less soluble pseudoephedrine salt because all the first part of the extraction is aimed at extracting everything *but* the pseudoephedrine. It's not really in a state to be easily translated, but I'm sure that it wouldn't be hard once the proper sequence and materials is established. |
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