The Vespiary
The Hive => Stimulants => Topic started by: kidclean on February 16, 2004, 09:15:00 AM
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Greets to all!
This is my first post, and I’m sorry it’s so long, but please be gentle with me...
I'm about to dream my first dream and have an assortment of questions. I *have* used TFSE extensively (as a former sysadmin, "RTFM" was a common saying of mine), so my questions here are either the result of having not found an answer, finding discrepant answers, or unclear answers. Also, I'm not completely new to chemistry; I have a few semesters of organic chemistry under my belt, albeit from 20 years ago. I don't want to use ghetto equipment, reading all the posts on stimulants board has convinced me to "do this right"--real glassware with quality chemicals using the long wet reflux method. With quite a bit of effort, I've managed to acquire 1 kg of reagent grade iodide crystals and .5 kg of reagent grade red phosphorus.
Without further ado, my questions:
1. I plan on using the meth I produce solely for self, no selling. I want to end up with ~7 grams of clean, methamphetamine hydrochloride. Is a two-neck, 500 ml 14/20 flat bottom flask adequate for the job? I plan on using one neck for a condenser and the other neck for a submerged lab thermometer. Is a 500 ml flask large enough? Is a flat bottom flask okay to use (as opposed to a round bottom flask--I plan on using a deep fat fryer for heating). What about 14/20 glassware for this size reaction, is it adequate? Do I need to move to 19/22 or 24/40?
2. Given that I plan on using a deep fat fryer/oil bath, how high should the oil be in relationship to the flask? Half way? What about the relationship of the flask to the deep fryer, is it okay/recommended to allow the flask bottom to touch the bottom of the deep fat fryer?
3. Assuming 14/20 is okay to use for this size reaction, what kind of condenser do I want? West? Friedrich? Liebig? Also, the 14/20 condensers apparently come in two sizes, 110 mm and 200 mm. I would like to be able to circulate room-temperature water and not have to use ice water, especially since I plan on refluxing for 48 hours. Can room temperature water be used? What type and size condenser to purchase?
4. I've never quite understood what should attach *to the top* of the condenser. A drying tube? A balloon? Nothing? My guess is that nothing need be attached as long as the condenser is doing its job properly.
5. I think I remember reading something in one of Uncle Fester's books a long time ago about not using pool acid as a substitute for good HCL (aq). Is this true? Believe it or not, I'm having a harder time finding lab grade HCL than I did finding RP and I!
6. Almost every post I've seen in terms of molar ratios/relative weights of precursors assumes matchbook- derived red phosphorus and tincture-derived iodine. My RP and I are reagent grade. Can someone please give me either molar ratios or, preferably, relative weights to use for this reaction for RP/I/E/H20?
7. Since I plan on doing a slow wet reflux, is making the HI in situ still frowned upon? Should I add the RP and I and water first, wait for them to react completely, and then throw in the E? Does it matter given a slow wet reflux? In what order should the precursors be added? Should the glassware or any of the precursors be chilled first in the refrigerator?
8. How important is grease for the ground joints? Any recommendations as to the type to use?
9. What about Keck clamps for the glassware? Are they needed?
10. I've just finished using ahgreich's Tetra Trap method on some 12 hour 120s. The pseudo looks awesome--needle like shards, white as can be. 71% yield, if my math is correct. Can someone verify this for me? I started with 12 grams of GUPS. I've got 6.99 grams of pseudo freebase. 12 grams x 165.2322 (molar weight of pseudo freebase) / 201.6931 (molar weight of pseudo HCl) = 9.83 g pseudo freebase theoretical. 6.99 g (actual pseudo freebase) / 9.83 g (theoretical pseudo freebase) = ~71% yield. Correct?
11. In terms of the pseudo freebase, is this okay to use in the reaction as-is? Do I need to convert it to the HCl salt first? I read where the reaction is even more exothermic if the freebase and not the salt is used. Is this a big deal? Will it require an ice bath initially? Does the use of the freebase vs. the salt have an impact on impurities?
12. I've read that PEG may have gotton through the Tetra Trap. How can I tell if this is the case? How can I remove it from the freebase crystals? Will a simple recrystalization remove the PEG? Any suggestions/pointers here?
That’s it for now (Thank GOD I'm sure you're telling yourself ;-).
TIA,
--KidClean.
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2: I would use a sand bath. I've never used oil baths, but they sound like a messy bitch. Zwitterton seemed to have had a preponderance of fires which might be related to his use of oil baths.
4: If you're running a dry reaction, probably a balloon. It depends how much HI gas the reaction makes. If it doesn't generate much, then you don't need to put anything on top of the condensor. I think the long wet reflux generates relatively little HI gas, so you should be fine with nothing.
5: No. Fester was full of shit on that one. He thought that the green color seen in muriatic acid was chlorine, which might replace the amine in the product. In fact, it's just metal salt impurities like nickel and copper.
11: The freebase should be fine, since it will form the HI salt in situ. I would probably convert it to the HCl salt first anyway, so as not to waste HI. I don't know anything about the tetra trap, but if it's just a solvent extraction, it should come out int he HCl salt anyway.
Regarding the tetra trap, I've always been a fan of straight to E. Fast, clean and easy. I've never had any problem with it, but I've heard that it doesn't work with all pills.
I hope you didn't buy your RP and I off Ebay...
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bees in the past hae done a lot of complaining about these when heating they are not as good as rbf.
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1. I plan on using the meth I produce solely for self, no selling. I want to end up with ~7 grams of clean, methamphetamine hydrochloride. Is a two-neck, 500 ml 14/20 flat bottom flask adequate for the job? I plan on using one neck for a condenser and the other neck for a submerged lab thermometer. Is a 500 ml flask large enough? Is a flat bottom flask okay to use (as opposed to a round bottom flask--I plan on using a deep fat fryer for heating). What about 14/20 glassware for this size reaction, is it adequate? Do I need to move to 19/22 or 24/40?
500ml flask is fine. 14/20, 19/22, and 24/40 will all work fine.
2. Given that I plan on using a deep fat fryer/oil bath, how high should the oil be in relationship to the flask? Half way? What about the relationship of the flask to the deep fryer, is it okay/recommended to allow the flask bottom to touch the bottom of the deep fat fryer?
Halfway is good. It is NOT recommended to allow the flask bottom to touch the bottom of the deep fat fryer, because that could cause overheating. Jack's experience with flat-bottomed flasks are that they are unreliable when they are heated directly on a heat source. Keep it about half an inch to an inch above the bottom.
3. Assuming 14/20 is okay to use for this size reaction, what kind of condenser do I want? West? Friedrich? Liebig? Also, the 14/20 condensers apparently come in two sizes, 110 mm and 200 mm. I would like to be able to circulate room-temperature water and not have to use ice water, especially since I plan on refluxing for 48 hours. Can room temperature water be used? What type and size condenser to purchase?
The condensers you mentioned will all work fine for the size of the reaction you want to perform. Room-temp water can't be used as that defeats the entire purpose of using a condenser. Ice water MUST be used as it will condense the boiled water vapors and hydrogen iodide back to hydrodic acid. The acid will return to the flask where it can continue reducing the (pseudo)ephedrine to meth. Use the longer condenser if possible.
4. I've never quite understood what should attach *to the top* of the condenser. A drying tube? A balloon? Nothing? My guess is that nothing need be attached as long as the condenser is doing its job properly.
If you can tolerate the smell and are not in a populated area, you don't need to attach anything on the top. Otherwise, attach a 16" punchball balloon to the top. It will inflate partially and stay partially inflated a certain amount for the duration of the reaction. The inflation occurs in the beginning of the reaction where the proper concentration of hydriodic acid is being generated from the red phosphorus and iodine. You're right, a big enough condenser, with ice water, will keep all the vapors in the lab setup. Don't use a drying tube.
5. I think I remember reading something in one of Uncle Fester's books a long time ago about not using pool acid as a substitute for good HCL (aq). Is this true? Believe it or not, I'm having a harder time finding lab grade HCL than I did finding RP and I!
I wouldn't worry. Regular pool acid works just as good in Jack's experience, and it's easy to get.
6. Almost every post I've seen in terms of molar ratios/relative weights of precursors assumes matchbook- derived red phosphorus and tincture-derived iodine. My RP and I are reagent grade. Can someone please give me either molar ratios or, preferably, relative weights to use for this reaction for RP/I/E/H20?
Assuming lab-grade precursors: 0.4RP/1.3I/1E/1H20.
Assuming OTC precursors: 0.7RP/1.6I/1E/1H20.
7. Since I plan on doing a slow wet reflux, is making the HI in situ still frowned upon? Should I add the RP and I and water first, wait for them to react completely, and then throw in the E? Does it matter given a slow wet reflux? In what order should the precursors be added? Should the glassware or any of the precursors be chilled first in the refrigerator?
Making HI in situ is not frowned upon. It doesn't really decrease the yield any or reduce the potency. You worry too much man! It doesn't matter how the contents are added to the flask so long as the last item is either the red phosphorus or the iodine.
8. How important is grease for the ground joints? Any recommendations as to the type to use?
It's defenitely recommended for complete insulation so the smell and hydrogen iodide vapors don't escape. I doubt that will be a problem, but grease them with any diuretic silicone compound, like Dow Corning High Vacuum grease.
9. What about Keck clamps for the glassware? Are they needed?
Are you making meth or doing a Grignard? No, they're not needed, but they're defenitely recommended.
10. I've just finished using ahgreich's Tetra Trap method on some 12 hour 120s. The pseudo looks awesome--needle like shards, white as can be. 71% yield, if my math is correct. Can someone verify this for me? I started with 12 grams of GUPS. I've got 6.99 grams of pseudo freebase. 12 grams x 165.2322 (molar weight of pseudo freebase) / 201.6931 (molar weight of pseudo HCl) = 9.83 g pseudo freebase theoretical. 6.99 g (actual pseudo freebase) / 9.83 g (theoretical pseudo freebase) = ~71% yield. Correct?
So, do you want meth or do you want to become a professional scientist? Lol, just kidding. You got it right.
11. In terms of the pseudo freebase, is this okay to use in the reaction as-is? Do I need to convert it to the HCl salt first? I read where the reaction is even more exothermic if the freebase and not the salt is used. Is this a big deal? Will it require an ice bath initially? Does the use of the freebase vs. the salt have an impact on impurities?
Freebase is a little bit more reactive. Use 82% the amount as you would the hydrochloride. That is because the molar weight of (pseudo)ephedrine freebase - 165 or around that - is 82% the amount of the molar weight of (pseudo)ephedrine hydrochloride - 202g. One mole of either form can afford up to one mole of meth - 149g. So 165g freebase or 202g hydrochloride reduced in under the same circumstances would result in an identical weight in meth. And the maximum possible yield is 92%.
12. I've read that PEG may have gotton through the Tetra Trap. How can I tell if this is the case? How can I remove it from the freebase crystals? Will a simple recrystalization remove the PEG? Any suggestions/pointers here?
An effective recrystallization could, but it's difficult. Letting the reaction proceed for 48 hours will break it down into compounds that an acid/base extraction will remove from the meth base.
Good luck! With the details of the questions you asked, I doubt you'll need any luck, though.
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Is a 500 ml flask large enough?
Yes for ~7 grams you'll start with 10g. 500ml might be overkill....250ml would suffice.
I see jackhole answered most questions, but in regards to the most important area(extraction), if the tetratrap was used alone without any method employed to remove OII gaak, then troubles could develope with the post-rxn workup.
Either read some of Geezmeisters latest posts on how he deals with OII gaak or after collecting you're pfed from the tetra trap, expose the xtals to a mixture of 10ml japandrier(active ingredients=petroleum distillate•naphthenic salts) and 100ml Tetra.
After the wash, single filter off the purple juice and dry the xtals! Re-extract using denatured alky or Isopropyl and pass through fine filtration collecting the pfed/alky for evap.
Once evapped, scrape up the xtals and proceed with several acetone washes to reveal pristeen clean snow white pfed.
Good Luck
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It's not better to do HI by addition of "RP+H2O+I2" and after add "E+RP" for the long Reflux ? !!!
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Yes for ~7 grams you'll start with 10g.
First time, you better start with 14g ;)
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If you really want to assure getting a full 7g's of recrystallized final product pad your starting amount by a factor of 3. Most likely you'll end up with a bit more than 7 but this starting amount should guarantee that you end up with the amount you might truly be expecting. A 20 or 21g reaction will still fly fine in that 500ml flask.
Once at the recrystallizing phase it's best to have more than you'd expect to end up with to start becuase the alcohol used in the process will still hang on to a decent chunk of it once the crystallization has taken place. What is retained by the solvents can of course be recovered but not as usably recrystallized goods from that particular session. They become additional stock for the next round of recryst.
Also if that flask is truly a free standing flat bottom a reflux reaction of this nature will run fine sitting straight on top of a hot plate with no need or extra hassle and hazard of an oil bath.
A common technique I didn't see mentioned, to deal with potentialy stinky gasses that would have some chance of exiting, is to run a length of flexible plastic hose/tubing from the top of the condenser(s) to the outdoors with the hose terminating into a bucket of stink absorbing kitty litter.
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It's not better to do HI by addition of "RP+H2O+I2" and after add "E+RP" for the long Reflux ? !!!
Maybe if you want to get a few percentages higher of a yield. Assuming you add the correct ratios, it really doesn't matter. Technically, it's better, but such a small improvement that you're unlikely to notice. And I'm talking in terms of the overall reaction behavior, workup, and finished product.
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Okie Dokie adnagi:
You are right....It's best to create HI first and then add E! ;D ;)
This process of creating HI first, reduces the risk of side rxns occuring that may not be favorable to yield or end result!
Therefore...add precursors in this order....
I2+dh2o, mix, then add RP, mix, then heat until gas is created. Bee ready to uncap and add E quickly soas to not allow the gas to escape!
I'm sure someone will PIPE UP with a correction... :o
(https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000488996-file_hpuw.gif)foxy2: >First time, you better start with 14g
(https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000488996-file_hpuw.gif)(https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000488996-file_hpuw.gif)(https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000488996-file_hpuw.gif)ChemoSabe: >Triple It
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Thanks to all the bees that responded.
Methymouse:
I will use a sand bath instead of an oil bath--makes sense...
And no, SWIC didn't buy his precursors from eBay. Not only has SWIC read the numerous posts warning against this, but SWIC actually has a good buddy doing time in the Penn right now for this very offense. He wasn’t too smart and ordered ephedrine from said auction site. Low and behold, US Customs, the local police and sheriff, and the DEA paid him a visit. He went down hard, having glassware and chemicals stored at his house. Tragic. Luckily the Feds declined to prosecute and left that up to the State. SWIC's friend has some advice to all bees. First, he warns against using eBay or similar. Second, he warns against having chemicals delivered to your house. If you absolutely must have chemicals delivered to your house, he advises several things. First is to know your regular postman and the person who fills in for him when he's on vacation--be wary of new faces. Second, be wary if the postman delivers at time that is different from his "normal" delivery time. Third, he warns against signing for any chems. SWIC's friend signed for a package delivered from any unfamiliar face and at an unusual time. Sure enough, it was a "controlled delivery" and search warrant used was contingent upon him signing for them chemicals. If he would have just refused to sign he'd bee with us today. SWIC's friend always strongly warns against having children in the house, unless you don't mind being charged with felony child endangerment and having Child Protective Services (or whatever they're called in your neck of the woods) trying to take your parental rights away (never mind if the child was actually endangered or not). Finally, SWIC's friend strongly cautions against having a firearm anywhere in the house. SWIC's friend had a gun, and though he never thought of using it against pigs, the DA slapped on a two-year enhancement to his charges. Bee careful!
Embezzler:
Thanks for the info regarding flat-bottom vs. round-bottom flasks. I knew that RB was the way to go if SWIC had a mantle, but he'll use RB anyhow now.
Jackhole:
Thanks for all the info. SWIC will use ice water in his condenser, but he's worried that 48 hours of refluxing will use a shit-load of ice. Oh well, time to invest in a commercial ice maker ;-). And a big thanks for the ratios, but SWIC has two questions regarding them. First, are the ratios you gave molar or equivalent weights? And second, are the ratios you gave for freebase or the salt?
Wareami:
Thanks for the info on the 250 ml flask. I'd prefer a 250 ml flask to a 500 ml flask for several reasons. Good to know that 250 ml should suffice. Thanks also for the info on recrystalization, OII GAKK and japandrier. I've seen japandrier mentioned in a few posts but have no friggin' idea what it is. I'll make it tonight’s homework lesson!
ChemoSabe:
Tripling ingredients? My God, my lab skills are rusty but not that rusty! If I get a 30% yield I think I should call it quits. Seriously, thanks for the info on saving the alcohol for a future round, and info on the flask.
Everyone:
I forgot one question. Obviously a deep fat fryer doesn't have built-in stirring, which raises the question: Is stirring necessary? How often?
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Obviously a deep fat fryer doesn't have built-in stirring, which raises the question: Is stirring necessary? How often?
Refluxing will mix the reaction good enough. You are doing a slow wet one right?
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If doing the WetDream(longwetreflux), stirring is not normally necessary as the rxn is a set it forget type rxn. It will completely reduce by itself. However, Ibee got into the habit of periodic checkpoints where it was determined that during these times, one could remove the condensor/balloon and stir. This stirring allowed any excess precursors that collected on the flask sides to be knocked back down into the jacuzzi where all the action takes place and they do the most good!
Checkpoints @ Every 8-10hours is sufficient!
Internal flask temps should not exceed 120°C
Japan drier can be found in paintsections of most home improvement stores or major paint suppliers!
(Must contain the to active ingredients listed in above post) ;)
It's use is mainly to speed the drying times of varnish and enamel paints.
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Japan drier can be found in paintsections of most home improvement stores or major paint suppliers!
So is Japan dryer a new wash solvent? Ware, Lets have a primer ;D on its usage.
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Here is a link to a thread where wildman Ware desciribes how to beat the Orange2 gakk down, with japtetratone of course!
Post 463438 (missing)
(wareami: "News Flasher Blue Streaker UP!", Stimulants)
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First, are the ratios you gave molar or equivalent weights? And second, are the ratios you gave for freebase or the salt?
Equivalent weights using the hydrochloride salt. If using the freebase, lower the amount from 1 to 0.82, k? Keep the other weight ratios identical.
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Foxy...in the beginning, there was lite! Than Ware came along.
Need I say more???
Ibee made the mistake of linking the Name of the new method to a .gif file that's no longer beeing hosted.
Do a search for the "Slanted Egull"(get it???slanted....japan??? okay...okay...I'll behave ;) ) and that will provide some more description on the latest quick clean from UP-AWE-NITE labs.
Thanx Gluecifer for Piping UP!
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Im a little confused about the nano scale,been away from the mad chefery for a bit and it just seems to be a lil cornfusin to me.been about 6 years since i fiddle faddled with anything but always thought you did 1-1-and a 3rd.Is it just diff for the nano sitiation?I dont think i lost that part of my memory.I did like the idea bout nano cause i know its like ridin a bike but its been a long time and i do remember when something can go wrong and you are dependin on it not to it does.So i like the idea of doin a lil trial to bring back the memory.Got a couple other things to ask bout but they will wait fer now.Thanks folks.. 8)
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Gluecifer has ran many nanos, and from personal experience, your basic ratios must be upped for quality gear or reflux longer if that is your bag. If using MBRP swim would recommend this ratio(also assuming I is from tincture), E:1,I:1.33,MBRP:,75. (if the MBRP has never been run, you can drop down to .50 if you are doing a LWR :) )
These ratios have given Gluey good results even in push/pulls.(AHHH yeah Gluey is still p/p'ing) I am sure that would equally as well if not better in a LWR.
If you will note swim did not give any water ratios, as they are directly proportionate to the time of the cook. For the push/pull you need 4mL/OZ of E. That came from the man Jacked.
Hey Ware, it is always Gluecifer's pleasure to PIPE UP!
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If your pseudo is from the generic 120's, you should expect it to contain orange II type gakk. You have freebase crystals from a tetra trap type extraction, and IMHO that will not give really clean pseudo. Your freebase crystals are likely heavy with PEG and orange II.
I have found that japan drier works as advertised in the extraction process to break down the OII gakk. The PEG can be attacked and removed from the crystals by the addition to the crystals of a little hot water...don't use too much. The crystals will reform and float, and should be filtered off and rinsed with a little cool water.
I might suggest that you dissolve the freebase crystals in tolly or xylene, wash that with a ten percent NaOH solution three times, then wash with water. If you get a grey emulsion in the water washes, be glad you did this step.
I do not take issue with any of the advice you have recieved. I might drop the water from 1:1 with the pseudo to 1:0.8; I would recommend a balloon, as the inital formation of HI gas outstrips the condenser's ability to condense all of it, icewater or not, at first. While I like cold water in the condensor at the start of a reaction, I do not use, nor have a seen a need to use, ice or ice cold water for the entire reaction. I change the water with fresh cool water if it gets warm.
For the size reaction you contemplate, I would recommend a smaller flask, a 250 would be fine, and recommend using a round bottom flask. I use an oil bath (actually a cool-to-the-touch deep fat fryer with a modified lid I can mount the flask to-- this keeps the heat in the cooker and the smell to a minimum, and provides a window to view the reaction. (I have done many of these reactions on a simple hotplate in a flat bottom flask, and have had good success with these also.)
I do not recall the temperature you intend to use. I recommend a temperature just below 100C.
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Well bees,
The time has come and gone. The final results (drum role, please):
From 25.92g of psuedo, SWIC has 16.52g of super-kick-ass, good-as-it-gets meth (after two recrystalizations)! SWIC is happy as can bee! If he did his math correctly, this represents a just-under 70% yield. Don't think that's too shaby for a second synth (and a first time non-nano synth).
SWIC couldn't have done it without *all* you kind bees and your helpful suggestions and answers to his newbee (and sometimes naive) questions. SWIC wishes to thank all of you! There are too many of you to mention by name, but SWIC will make one exception--Geez.
Geez, your answers were always right on the money and SWIC doesn't think he would have succeeded without your advice. You *da man* in SWIC's book, bro!
Now, off to go get some KOH ;-)
Adios everyone,
--KidClean.