Author Topic: Processing 1 Mole Ketone Using Nitromethane  (Read 4111 times)

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baalchemist

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Lab Bitch should just shut the fuck up.
« Reply #80 on: January 04, 2003, 05:31:00 AM »
Lab Bitch should just shut the fuck up. People dont give a fuck about your views on the DEA or anything else for that matter. Go hang out in a teen chatroom and preach, they still may be reachable. This is a chem board discussing production in case if your fuckin' blind or in this case, just plain stupid.


madprosr

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baal, you 'da man even if you freeze your...
« Reply #81 on: January 05, 2003, 10:29:00 AM »
baal, you 'da man even if you freeze your safrole upside down! power to the people!

anyway, my apologies to abacus who's 6% solution i interpreted as grams MeNH2/grams MeOH. if abacus says he gets 3mol MeNH2 in 1400ml MeOH (ie 1400ml of 2.14M solution) then i believe him completely.

swim ran his synth at 1/10 scale using 120g of 15% nitro in a 500ml flask.
15.9g of pretty thick flashing were cut in thin short strips and curved slightly.
the nitro contained about 100ml MeOH already so the Al was amalgamated in just 50ml MeOH (undistilled, yellow-bottle) with sufficient HgI2 to cause immediate bubbling. as the nitro was dripped down the condensor over an hour a cold water bath was needed to permit continued dripping. the Al swelled up with sludge rising partially out of the MeOH and three times ~25ml MeOH was added and the flask shaken to redistribute the sludge.
after reflux stopped another ~15ml MeOH was added and the flask heated to slightly below reflux for 4h. it was left stirring overnight, but the top layer congealed at some point. in the morning heat then shaking were applied to get everything moving again. swim observed that the square corners of many pieces of Al were now rounded. the mix was heated to slightly below reflux again for 2h, until most of the Al was gone. swim got tired of waiting and added 19.6ml 50% NaOH which heated it up somewhat. he then carefully distilled 220ml MeOH from about 400ml sludge until the castor oil got thick and it bubbled up.

so it was a messy amalgam, but swim measured MeNH2 concentration at .00137mol/ml, ie .3014mol total. ie 220ml of 1.37M solution. this is starting from .2951mol MeNO2 if weight and concentration were exact. but swim knows he went a drop over as he titrated 1ml using 1.65ml of 2.7% HCl because the pH went from 8 to 2 with that drop.

and nothings exact, but swim got damn near quantitative yields at 1/10 scale with 15% nitro.  :P

swim bets if you use 20-30% nitro and start with more MeOH it will run great.

however, swim tried using 8% nitro he distilled (21.6g nitro) in a 400ml reduction and got bad (28.6%) yields. it was stirred for 36h with occasional heating but the Al did not break down. it was strained out. this sucked...

swim thinks his last reduction of 96g of 15% nitro yielded only 31% because he added base only 1h after finishing the nitro drip. the reflux had stopped, but the reaction was nowhere near done, and heating it all night after that did not complete it, only drive off some MeNH2. don't basify too soon with thick Al and a small reaction.

anway, the .3mol MeNH2 works great:
swim used .1mol in a 5.4 gram ketone reduction ala Os and got 4.6g hcl salt.
used 2.55g Al and 75ml MeOH (undistilled, yellow-bottle). heated and ran overnight. only 10ml of 25% NaOH were used to reach pH 12, even though Os's amount is 200g NaOH/ 55g ketone. extracted 3x 40ml toluene but the MeOH mixed completely with it. used alot of brine, careful rocking, to separate the MeOH without emulsifying everything, then washed the toluene. back extracted the alcoholic mother liquor + first washes + all emulsions with 10x 20ml toluene, until it stopped pulling light yellow color. (yeah, swim knows its not supposed to be yellow, but he didn't separate the iso from ketone when using a new 250micron pump for the first time). anyway, he gassed and filtered 4x, overgassing the last time, turning that last crop of crystals pink, which was fixed by an acetone wash, yielding 4.6g before recrystallization.

so kind sirs, does swim really need to add 10-20g NaOH to a 5.5g MeNH2/al/hg, definetly giving pH 14, possibly turning the sludge black, in order to keep the MeOH from mixing completely with toluene?
swim figured his was a problem of density, MeOH being .81 and toluene .87, ya gotta add h2o until the MeOH/h2o is heavier. how is it you guys get toluene extraction to work so easily???
swim is almost ready to try xylene, or some friggin' dcm. he just prefers to pipette solvent off the top, rather than having to vacuum filter the sludge. he supposes with two filter-funnels (one evil, one not) this is no problem.
or is it the dang undistilled MeOH, and using it for the h2o source???

anyway, now that you have gotten this far, i have perhaps a very good idea...
1) distil safrole+iso after KOH isomerization as a mixture from 70-80C with your overpowered vacuum pump.
2) throw the mix on an equal volume of frozen safrole in the freezer for a day.
3) pour off pure iso with the safrole frozen out
some iso will stick in the container, no big deal...

so what do you guys think? swim's going to treat some mixed safrole/iso this way then do a bp test for purity shortly. anybee know for sure already if it works?

Rhodium

  • Guest
No go
« Reply #82 on: January 05, 2003, 02:32:00 PM »
trans-Isosafrole melts at 6-8°C (see

Post 385627

(Rhodium: "Isosafrole Physical data", Newbee Forum)
) so you cannot separate safrole (mp 11°C) and isosafrole by freezing like that.

madprosr

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Rhodium, swir's seen trans-iso freeze from a...
« Reply #83 on: January 05, 2003, 11:39:00 PM »
Rhodium, swir's seen trans-iso freeze from a mixure of both isomers? At what temperature?

last time around, swim isomerized 30g then added the pure iso vacuum distilled from 150-158C (sassy forerun was at 140-144C) to 15g safrole crystals in the freezer for a day. swim recovered 26g, so it doesn't seem that significant amounts of trans-iso froze out.

i guess swim is just looking for a way to use a lower distillation temperature, without adding a fractionating column.

what swim wonders is whether the sassy freezes out 100% or not???

wacko_reaco

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got to get back in on this act
« Reply #84 on: January 06, 2003, 04:18:00 PM »
if it don't hurt the reaction and you are good at purifying the product (distillation, re-crystallisatin, chromotography, whatever), then why bother, that's all, rhodium your boss, if you want me to shut-up about this then fine
lisa 'i did it my way' minnelli


carcrash

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Heh try 3/8 aluminum rod
« Reply #85 on: January 10, 2003, 01:03:00 PM »
Sure you need to add a bit of heat but its gentle and no boil over.  You can add all the nitromethane at once. Longer run time but way easier to cut that into a few pieces than cut up flashing. Chop saw :) 4 pieces fit in the flask and hit the 162 grams.


carcrash

  • Guest
Nevermind dont try 3/8 rod
« Reply #86 on: January 23, 2003, 10:34:00 AM »
Unless you have a disposable reaction chamber.  Probably lost the flask.


Wargasm

  • Guest
A note on Al flashing
« Reply #87 on: January 25, 2003, 12:49:00 AM »
There was some trouble making this procedure work, which I just figured out (I hope).  Some Al flashing has a very thin coating of plastic on it, I presume to prevent corrosion against the elements.  This coating, IME can affect the rate of the reaction, if it works at all, and generally screw things up.  This was discovered on inspection of the amalgamated Al squares, which appeared to have been reacted on the corners only.
To deal with this problem, I am going to try a wire wheel on a drill before slicing the Al up.
you can tell if the Al is plastic coated by scraping it with a knife.  If it is coated you will find a small residue coming off.
I hope this helps anyone having problems with this reaction.



BlingBling

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Coke cans
« Reply #88 on: January 25, 2003, 01:57:00 AM »
Can someone try this with coke can's and report back? I never read one post where someone had success with soda can's, yet there has been alot of "use can's" talk in the past.

raffike

  • Guest
Cans are coated with paint outside and thin...
« Reply #89 on: April 14, 2003, 04:15:00 PM »
Cans are coated with paint outside and thin plastic coating inside.Raf has tried to to amalgamate one of those and it didn't work.


quantum

  • Guest
way to go abacus :)
« Reply #90 on: July 02, 2003, 02:45:00 AM »
yep its fool proof im a fool and it worked perfectly :)

hehe and I used realy thin foil for the nitro and it worked
a dream :)
not a single problem just took my time adding the nitro
and ran my aspirator water pump through my condensor so a larger volume of water would go through my column.
admitadly the liquid was halfway up the condensor and
the reflux was one winding off the top but the condesor
is only a little 200 mm so all in all I am very pleased.
personaly I think (it is a though so please corect me if I
am wrong)
that so long as you control the reaction the harder you run
it the better.

next any one done an aminomerciation of safrole.

will this work out for asarone.

keep up the good work guys and girls thank abacus.