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Hive BB  Chemistry
Discourse  Frustrated
& Fucked
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| Author | Topic: Frustrated & Fucked |
| Bankrobber Hive Bee |
 posted 02-29-2000 10:24 AM 
SWIBR dreamt AL/Hg and allowed to many variables,(got way to cocky,don't ever let dreams of the past make ya think that you can't run into any mistakes) henceforth comes the frustration. Any input greatly appreciated.Somebody Who Isn't Bank Robber did Al/Hg normally, put 200g not-methylamine in 400ml denatured alcohol and neutralized w/ NaOH(didn't vaccum filter, call swifc crazy, but the salt and excess NaOH is worser on stirbar than aluminum sludge, it stops it up in a second, vaccum filter w/o not-methylamine loss, I think you only lose a significant amount at post-reduction during vaccum distillation), added 80ml ketone(legal reagent), added 40g aluminum foil(usually does 1g aluminum per g of k, but this wasn't one of the fatal blows), than finally in her dream she saw .5g of mercuric chloride added(normal)! All I was told was that it went well until she dreamt reduction was over(reduction went fine, but heres were her fun starts), first she adds 50%NaOH solution and waits for supreme seperation, that individual than distilled down all the collected yellow solution(yellow layer rests above aluminum sludge layer),and the top polymerized/crap layer(layer directly above yellow layer, what is this crap), but only distilled until it was beleived that all alcohol was gone,she still had somewhere between 500-1000 ml left(usually distill until residue is very evident, SWIBR thinks that this might have been one of her major variables). Than she took the top layer of crap above the yellow layer(I thought that this was were the not MDMA layer came out from the distilling, a lot of times your layer seperates during distillation and that is product)and distilled it to yield about 30g of a yellow oil(she said she believed this to be to be ketone, fuck just when she thought she was smart, she finds out that she has a lot of learning to do, regardless of past experience), and put into dry toluol(toluene) and tried to gas, no dice(damn probably was legal ketone, arghhh!), THAN TRIED TO DO A/B on YELLOW LAYER(knowing whatever is there is in yellow layer as usual,don't forget I didn't distill till I got residue, just till she distilled off all of alcohol she beleives, arghhhh!)with red devil lye(damn she said that was all that was there in her dream, what a fool, should have waited for NaOH pellets like normal,never used red devil lye), plus she added it in just straight, no solution(fuck pride, you can always fuck something up, SWIBR has since learned it is better to demonstrate patience than to rush and make a fool of yourself, I'm embarrassed to even post this but felt it had to be done, to find out what went wrong and to demonstrate that it is usually lack of patience that makes a lot of people fuck up, don't convince yourself that you know everything because there is a good chance you dont), solution went from original color to a brown solution in a few seconds(cloudy to but not the good cloudy/pink color that SWIM is accustomed to), tried to extract w/ toluol but it went to the bottom(what the fuck, I know this may not be a good enough description, but please display possible variables, any knowledge greatly appreciated!). This Sucks Big Time,SWIBR! |
| Bankrobber Hive Bee |
posted 02-29-2000 10:27 AM
OOPS!meant to say this time dreamt of using 1g aluminum to 2g ketone(legal reagent). I apologize for my incompetence! |
| Bright
Star Hive Bee |
posted 02-29-2000 12:44 PM
1. How was the ketone made? 2. Was it distilled? 3. Relative to the distilled forrun ... what temp did the 'ketone' come over? 4. You just dumped all of the reagents into the pot at once? (Foil, MeAm, Alcohol, Ketone ...) Want to practice the reaction? Practice on some nitro-methane. Seal up a round bottom flask ala, Osmium, and direct the gas into an alcohol bath. Bubble away. PS- 1g Al to 2g of 'k' is an acceptable ratio. |
| Bankrobber Hive Bee |
posted 02-29-2000 01:44 PM
Bright Star ketone was made via benzo-wacker, it was distilled at 189-200c, and was turned into a bisulfite w/sodium metabisulfite, 1 week later it was regenerated to it's oil form w/ NaOH(wich works easily everytime w/ good stirring and heat addition), extracted with toluol, and toluene simply distilled off. SWIBR put 200g methylamine into 400ml denatured alcohol, added 225-250ml dh2o, than basified with 110-120g NaOH(this time SWIBR didn't vaccum filter excess salt/Naoh, in my opinion salt/naoh makes it harder to stir, and vaccum filtration doesn't effect methylamine that much, I think you only lose significant amount of methylamine during post-reduction during vaccum distillation, you get a lot of white smoke/vapor wich only stays for awhile unless you have high ph 12-14 than you get a lot of white smoke), than let stir for five min. to form Schiffs base. After five min. SWIBR added aluminum to flask, and finally .5-.6g mercuric chloride and just swirled for ten min. until amalgamation was evident, attach regular West condenser(whats your thought on what condenser to use?) and let boil for 4 hrs.(oh yeah never mag. stirred except in beginig to form schiffs base, every 30min just take condenser off, immerse in ice solution, than swirl for 1-2min. reattach condenser and commence to boil/reflux until there was no turbulence and temp. went down to 27-28c, aluminum completely amalgamated. Somebody Who Isn't Me still has three containers of reaction(two brownish color, probably from lye addition, and one has the oh so popular yellow tint, how theoretically can this be salvaged, remember that red devil lye was used w/o Dh2o,solution is heavily diluted w/ h2o, and it doesn'y look good). Solution was a different color prior to turning brown from lye addition. Thanks for taking the time to read post and respond back BS, your kindness is duly noted!
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| Osmium PimpBee |
posted 03-01-2000 03:54 AM
1) Your reaction contains too much water. Use much less. 2) Your reaction uses not enough solvent. Use more EtOH. 3) Add the Hg salt BEFORE all the other chemicals. Hg salts are insoluble in basic pH. I know it works, I did it once too, but amalgamate without the other shit already in there. 4) When you choose to filter the Al sludge, no Freebase layer should be visible, it should still be soluble in the reaction solvent, otherwise it will be absorbed even more by the sludge. Wash, maybe even boil the Al sludge with more EtOH, it contains LOTS of freebase. (This does apparently not happen when you use the strong NaOH sludge dissolution) 5) Do a A/B extraction dammit! |
| Bright
Star Hive Bee |
posted 03-01-2000 09:53 AM
You boiled the solution? Denatured alcohol boils at 78C. And why so much water ... Water reverses the imine condensation process! 'You must not let the temp get above 60C' -Bright Star If you can distill.. why the %!@#$%! are you bisulphiting? Not only is it a yield killer, but it's USELESS IMHO. And listen to Os's last post! The man knows his shit! And ... choose a method ... Os's, mine, Ritter's, Shulgin's ... it doesn't matter ... and FOLLOW IT VERBATUM! |
| Bankrobber Hive Bee |
posted 03-01-2000 10:45 AM
Bright Star your the greatest(well after Osmium of course), how does the bisulphite bad, it removed the green color to SWIBR's not ketone making it more pure, SWIBR needs real clean not-ketone to do the NaBH3CN or else SWIBR will just wind up w/ 30-40% yields. BR aint trying to dispute w/ you I just thought that this was a good thing because the thought of having to distill not-ketone x2 sucks, BS can the not-ketone be recovered from the benzo-wacker after mega washes(naoh wash x2, sodium bicarbx1, Naclx1, dh2o x2,and finally vac filtering excess hydroquinone) with sodium metabisulfite? Serious Bright Star your far more intelligent than myself, but I can't help but think of the possibilities of doing the benzo-wacker and just bisufiting after vac filter and washes, what do you think? Plus it's hard to tell if you got not-safrole in not-ketone during vac distillation, call me a fool but a few drops seem to come over at temp. near not-ketone but different than regular sass temperature, this is enough to screw w/ yields in certain reaction(somebody who isn't me wont be trying NaBH3Cn reduction very soon, and previous exp. shows one drop of any contaminant will give the "world famous" 30-40% yield, wich is dick, compared to previous exp. w/ Al/Hg) One time SWIBR added 4oz of sodium metabisulfite to 500ml water, than added 100g of not ketone and stirred, after bisulfite added, it was busted up w/ NaOH, and it didn't contain that green color just yellow(after distilling x2 SWIBR wound up w/ exact same color), and it appeared visually that maybe 5% was lost. Further feedback from Bright Star or Osmium would be greatly appreciated, thanks for taking the time ta post, shine on you crazy diamonds! Bank Robber |
| Osmium PimpBee |
posted 03-02-2000 04:33 AM
Seems like your bisulfite solution is too diluted. Make a real concentrated one, with undissolved crystals on the bottom. Use only the overhead solution of course. Fiter the precipitated bisulfite-ketone compound, wash it with ethanol, maybe even some ether, and decompose it with NaOH or HCl. Extract, dry evaporate. |
| scwam Hive Bee |
posted 03-02-2000 11:22 PM
Bright Star, Today, someone was refluxing meoh in the al/hg. Is there a problem w/this high temp? I think Osmium used refluxing on Etoh. The addition, even extended over an hour was done in a sep funnel through a rubber stopper into the 2liter flask. The Ketone/Nitro/Meoh solution in the sep funnel was being bombarded with gasses from the reflux. Im assuming that MeAm gas is being recondensed into this solution which drips back down into the boiling flask again. So, with this in mind, after the addition, and with the al/hg still rapidly boiling (~1hour after addition started) the sep funnel was filled with 800ml of Meoh to be bubbled while in the process. Kill 2 birds with one stone. This MeOh solution stinks of amonia now and is still crystal clear. Am I write in the above that that solvent will be good for future runs and when refluxing it up into the MeOh, does this mean Methylamine is being lost from the al/hg? It was assumed that some was being lost and taken into the clean MeOH above, so about 200 more ml or MeOH was added directy from this saturated solution at 1.5 hours into addition, boiling was still pretty much vigorous. |
| Bright
Star Hive Bee |
posted 03-03-2000 11:38 AM
Bank - The NaCNBH4 ... (or however it goes) .. is an effective method if you just want some product. If you do it right then you get consistant ~35% yields. For shits and giggles (once), not-me tried the bisulphite, and in the purification procedure, I lost 30% of my ketone. FUCK! If you really want the ketone pure ... distill it twice. But one good distillation run, would be pure enough fo the Al/Hg. During Vac Distillation the saf, and ketone should be separated in temp by 20+ degrees C. Do a vacuum distillation of your sassy oil, and then you'll know where it comes over ... then do the same distillation on the ketone ... You'll see where it comes over. Scwam - The temp thing has been a re-occuring subject for many moons.
Not-me has actually gotten ketone at the EtOH reflux temp ... but it
wasn't much. All the alcohols work real well in this reaction. MeOH, EtOH, IPA ... etc. The reason not me likes the MeOH is because it refluxes at ~64C. PERFECT. The down side of using the MeOH is that the work-up is harder ... the separation at the end of the reaction is much more difficult ... Others use IPA .. With IPA you have to watch the temp ... but the Work-up is much easier. The solvent you are using *should* be OK ... but how are you going to quantify the MeAm in the solution? I guess if each time you just add the right amount of MeAm it shouldn't matter ... but ... its just not very anylitical. The refluxing liquid in your solution is prolly MeOH. The MeAm is a gas, and unless you have a 400mm condenser with ICE water running through it ... you aren't going to condense much of the MeAM gas ... Hope it helps. I'm gong skiing! See ya'll in a week! |
| KrZ Hive Bee |
posted 03-03-2000 12:15 PM
That damn HCl pH adjustment was the problem with the NaCNBH3, if you just use GAA for adjustment, stir the reaction, and do it under nitrogen you can get the reported yields. Although you still need that big ass 1kg excess of MeAm•HCl. |
| bla
nka Hive Bee |
posted 03-03-2000 04:40 PM
OK, in my experience, very careful monitering to keep temps between 40-50 gave the best yields. Before doing anything, I prepared all the reagents. I then amalgated the foil. Dumping in everything at once is a bad idea. It is a shortcut that increases your chances of failure. Follow BS exactly, word for word. He spells it out for you step by step, with details. 1 ditillation is enough for me, and it always worked fine. In BS's step by step synth, you know exactly when the MDP2P comes over. It is (under vaccum) 25' over what the safrole comes over. Until you get used to doing this, going by this rule can help you determine whether you are getting MDP2P or safrole. If you want the best yields, i would go for labtop's NaBH4 reduction. I have got the best results with this method. If you take the time to understand and do exactly what he says, you can get ~90% yields. |
| Bankrobber Hive Bee |
posted 03-08-2000 05:50 PM
O's you previously stated that to much water is being used(200-250ml dh2o used as source of h2o for 200g methylamine basification,80ml ketone being processed) isn't this in sinc with your original al/hg write-up, in it 40%methylamine was used, I know it's just me, but I just wanted to get this straightened out(forgive my shortcoming's O's). How much ethanol is used per 40g of not-ketone, in the original laboratories amidos write-up they used 200ml ethanol per 40 g of not-ketone, and they also sported a 25% methylamine solution as opposed to 40%(I know 40% is the best of the two though). And what would the amalgamation be best done in(dh2o,ethanol), br thought it didn't matter, but now she see's different. Please correct me on these scenarios, SWIBR is sick of good/bad results(damn shuligan's always worked, no prob's) from variables she's not even aware of, please for the sake of education pass on the info.Thanks O's(or BS), That Nigga Bank's |
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