Author Topic: Processing 1 Mole Ketone Using Nitromethane  (Read 14678 times)

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yinga

  • Guest
Re: They might not be able to get the IP from ...
« Reply #60 on: December 06, 2002, 06:56:00 PM »

They might not be able to get the IP from this website, but if I understand correctly, they can trace it through your ISP router.




Even if they know you are accessing the hive, they are unable to tell one username from another because of the ssl encryption.  The only way they could determine what user you are from your ip would be by checking the time of post on the hive and comparing that to the time your ip sent information to the hive.  To prevent this problem either all packets sending and receiving need to be same size (they may already be, I dont know, does anybody know for sure?) or all posts need to be queued until a certain number of posts, say 10 or 20 are made before the hive software updates the message board, each post having the same time.  Even in the case of the latter it would still be possible to deduce which username you have (provided you make enough posts over a long enough period of time) by the process of elimination, so the former is definitely the best solution.  Of course,what are the chances that your ISP (or your ISP's ISP, etc.) would deploy this method.  If they know an incriminating post was made during the time you were accessing the hive there's a one in however many people were online at the hive at the time chance it was you (provided posting and reading packets don't differ).  Actually I do wonder if "post" packets differ from just "read" packets or PM packets.  If they did the ISP could easily tell the exact time each time you made a post, then look at the message board and find the username that made a post at each of those times.  If nobody knows if they do differ or not swim will sniff the packets and find out.  But I'll get back on topic:  good work abacus ;)


terbium

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Off topic.
« Reply #61 on: December 07, 2002, 02:26:00 AM »
The last half dozen or more posts have been completely off topic. Start a new thread if you want to continue this off topic conversation.

Baseline Does Not Exist.

lab_bitch

  • Guest
No life is better than life in prison
« Reply #62 on: December 07, 2002, 02:34:00 AM »
I'm mainly talking to people in the U.S.  It's a simple precautionary step.  You don't go around telling everyone in your town what you do, so why should you post this information on the net?  The NUMBER ONE reason that people get busted for anything is that they didn't keep their mouths shut when they should have.  Generally, if something doesn't need to be said, then don't say it.  I just know too many people that have fucked up like this and are now serving 10 year sentences in state prisons.  Whether or not posting that you make kilos of product is a real risk, why take it if it's completely unnecessary?  Sorry if I'm being a little paranoid, but in the U.S. this shits no joke.  If they want to fuck you, then they will.  Even Osama and friends (FUCK THEM!!!) can't avoid our security.  In fact, I wouldn't produce shit like that in the U.S. to begin with.  Talk to someone who's spent the past ten years in prison and get their opinion.  Performing research is one thing, but the second you start spitting out mad product, the question does not become whether you're going to get caught, but when.  That game is no joke!  Sorry if I'm making anyone trip out, but I may just be doing you a favor.

madprosr

  • Guest
in a dream, the largest flask swim has is 500ml.
« Reply #63 on: December 11, 2002, 10:03:00 AM »
in a dream, the largest flask swim has is 500ml. so he used it to reduce 144g 15% MeNO2 using 20g extra heavy duty foil. (for a 21g ketone amination) it ran out of control, climbing up 2 200mm condensors, but swim chilled it out running cold water directly onto the flask as needed. lots of hydroxide sludge was produced.

dammit, he soaked the hotplate and now the heat won't switch on only stirring. grrr... it was his nicest piece of equipment and switching the fuses inside doesn't help... grrr...

so unless it magically revives after drying out overnight swim can't distil the MeNH2. he read the methylamine faq and brightstar's synth on Rhodium's, but can't decide-
1) should he titurate the ~150ml of MeOH + castor oil + 11.8g NaOH + 15ml h2o to find out the MeNH2 concentration and add it directly. he sees a problem putting NaOH into the reaction, he could neutralize it with HCl possibly.
2) should he just extract 3-4x 20ml dcm, add HCl until slightly acidic, and (this is a worst case scenario) boil off the dcm and trace h2o on the ol' stove. then weigh it and do like the Os man says  8)
so, uhm, methylamine responds to standard a/b extraction like all the other amines, right?

please advise, otherwise swim can just run 5g MM type reactions with some previously distilled 8% MeNO2. but a smooth MeNH2/al/hg would bee so much nicer.

needless to say, this is only a temporary handicap...

BlingBling

  • Guest
>>needless to say, this is only a temporary ...
« Reply #64 on: December 11, 2002, 10:54:00 AM »
>>needless to say, this is only a temporary handicap. but he's got to run an amination now with what he's got.

Well then you have your answer. This thread has nothing to do with your problem. You should of posted in the stupid mistakes thread instead. Pouring water over the flask with an electric hotplate below?! 

Sober up when working. It could save your life, or someone elses.

madprosr

  • Guest
more concisely
« Reply #65 on: December 11, 2002, 11:05:00 AM »
after one basifies the post nitromethane reduction sludge, can one extract the MeNH2 with a nonpolar solvent instead of distilling it?

as for swim's idiocy, sure he put it on a cold water bath, then it started running away again anyway. whatchagonnado??? i suppose this is old news to bees used to running 25g MM aminations... in 2L flasks, heh.

abacus

  • Guest
Thicker aluminium
« Reply #66 on: December 12, 2002, 08:50:00 AM »
For the last time, I said to use THICK aluminium greater to or equal to 0.3mm thick.  Geez, its like playschool, you have to repeat everything about a million times.

Don't use heavy duty foil, its way too thin which will cause the effect you described unless you add it very SLOWLY.

The methylamine is highly soluble in aqueous solutions, even if you basify most of the methylamine will stay dissolved in the NaOH solution and wont go into DCM. 

Your only way forward that I see is to distill out the methanol with some methylamine from the flask. That way you know you leave any unreacted nitromethane behind (too much unreacted nitro may stuff up any ketone animation attempt).

Abacus

madprosr

  • Guest
swim thought it might work on 1/8th scale with ...
« Reply #67 on: December 12, 2002, 10:30:00 AM »
swim thought it might work on 1/8th scale with extra heavy duty foil...

anyway, he realized MeNH2 is soluble 10:1 in water, so lacking a hotplate, he added some ceramic chips and distilled it on an oilbath on a gas stove. the MeOH came over starting at 70C (past the 65C where 8% MeNO2 comes over, whew) and climbed to 80C at which point the castor oil got too thick and heat was removed to stop the excessive bubbling. 30ml of water and oil in two layers remained.

uhm, i know this was slightly dangerous, can someone quantify how much?
abacus, how do you know for sure any nitro will be left behind by distillation?
just by observing that adding the MeNH2/MeOH to an amalgam is not exothermic?

tituration determined the concentration was 1.5%, about 1.5g total in 125ml MeOH. he suspected yeilds would suck as the voluminous purple sludge looked to be about 400cc. this was from a 21g MeNO2 reduction with 20g Al and about 300ml MeOH. the sludge held 200ml of MeOH even after filtering with aspirator vacuum.

ah, well. practice makes perfect. the MeOH was super-wet it turns out (crack in the nalgene bottle). so the 4ml of h2o added with the MeNO2 sure didn't help things out...

wacko_reaco

  • Guest
are you guys for real
« Reply #68 on: December 12, 2002, 09:48:00 PM »
this must be the easiest synth ever posted, if you are haveing problems just run the MM nitro synth without the ketone then distil before basifying, voila 6% MeAm in MeOH.
I have now performed this method three times (with 50, 50 and 500mg (ha ha)) and it is killer, important though to stick to the instructions.
Congrats ab babe for the no brainer method.
I use foil in the ketone reduction step and a water bath set on 70C (reaction temp approx 60C, rxn time 8hrs)

wacka wacka wacka

abacus

  • Guest
Finally
« Reply #69 on: December 13, 2002, 07:48:00 AM »
Finally!!!  Thanks wacko

Also, I forgot that nitromethane and methanol forms an azeotrope so distilling doesn't necesarily leave the nitro behind.

Madprosr, you have a long long ways to go, pm me if you want specific help

Abacus

hCiLdOdUeDn

  • Guest
Tests for nitro?
« Reply #70 on: December 14, 2002, 01:07:00 AM »
I know it really doesnt matter with nitromethane being in the methanol but is there any test for unreacted nitromethane from post-distillation of contents? I have about 1L of some distilled suspected 6% methylamine/methanol which smells strongly of methylamine but I want to make sure there isnt any nitromethane because nitro makes an 8.3% azeotrope with methanol.

Sink or SWIM

abacus

  • Guest
Pour in into al/hg
« Reply #71 on: December 14, 2002, 02:49:00 AM »
Pour it into a flask with some amalgamated aluminium.  If it heats up there must some nitro in there. 

I never got any nitro distilling over when I did as it was always reduced to methylamine. 

So amalgamate say 30g aluminium, pour in suspect methylamine solution and see if you get any temperature rise after a few minutes (you probably won't), if not, then pour in the ketone (around 120g) a little water and gently reflux and away you go.

Abacus

wacko_reaco

  • Guest
the shit should really stink
« Reply #72 on: December 15, 2002, 05:44:00 AM »
-thats the best confirmation in my book, if your are worried about lesser concentrations then use more of the MeAm/MeOH as excess of this reagant will in no ways hinder the rxn. Also in my previous post i said i used foil where in fact i meant flashing, 0.3mm, sliced into ~0.5-1mm strips using a gulotine (spelling), for cutting up decent amounts i suggest everyone buy one, you can thinly slice 1kg of aluminium sheet in about 15mins if you go hard or 30minutes if your a a slacker, much better than sissors.
The only drawback for some with this method will be the neccessity to redistil the freebase, but you all should do that anyway as the differnece is noticeable.  And now that we don't have to bother distilling the sass or the iso you should definetley redistil the freebase.

wacka wacka wacka

Rhodium

  • Guest
What's this talk? Are you proposing to skip both ...
« Reply #73 on: December 15, 2002, 10:05:00 AM »
What's this talk? Are you proposing to skip both the distillation of sassafras AND the post-isomerization mixture? To skip one of them is not good, but skipping both is completely fucked up!

If you haven't run into any problems doing that, then you must be extremely lucky with your source of sassafras oil, as most types contain 10-20% terpenes, and only 80-90% safrole. Those terpenes will easily be carried through the isomerization, and some of them will undergo peracid oxidation forming who-knows-what. These impurities simply MUST be removed by fractional distillation before doing the peracid oxidation, preferably by distilling the sassafras oil before isomerizing, but at least when distilling the isosafrole after the isomerization.

Doing anything else is irresponsible, if not downright stupid in some cases. Remember that you are making something that people are going to ingest!

hCiLdOdUeDn

  • Guest
YES, You are totally correct.
« Reply #74 on: December 15, 2002, 04:25:00 PM »
YES,

You are totally correct. SWIM has tried a epoxidation with undistilled "suspected" isosafrole/safrole/NaOH Mix and it did NOT work at all (couldnt get any epoxide or glycol to form). (AS EXPECTED) But swim just had to try.

It is essential to purify EVERY step of the way to maximize yields and minimize impurities! SWIM had to find out the hard way  :-[

Sink or SWIM

Semtexium

  • Guest
DAmN!!!
« Reply #75 on: December 15, 2002, 08:19:00 PM »
That has to be one of the only times I've ever seen Rhodium get so pissed off as to swear!!!  Don't piss off the Chief bee you BASTAGES!!!

::)  ;D  :)  :P  ;)     Mean People Suck     ;)  :P  :)  ;D  ::)

Rhodium

  • Guest
I have washed my keyboard with soapy water now...
« Reply #76 on: December 15, 2002, 10:20:00 PM »
Pardon my french, but just minutes earlier I had in

Post 389594

(Rhodium: "Shortcuts can easily become detours", Methods Discourse)
strongly argued against Ruth's proposal to skip distillation of isosafrole because he could not afford spending time on that, as he considered himself a "production chemist", and now this outrageous statement that one should take crude sassafras oil and subject it to isomerization directly followed by performic oxidation to MDP2P without any isolation or purification at all of the intermediates - and all this without any purity checks.

It is bad enough if Mr Ruth actually practices such sloppy lab technique in his garden shed, but coming here and suggest that other people should lower their standards to his level - then even I become somewhat agitated...  ::)

BlingBling

  • Guest
heh
« Reply #77 on: December 15, 2002, 10:26:00 PM »
Karma patrol catches up with people like that. No worries.  ;)

madprosr

  • Guest
still not quite up to one mol...
« Reply #78 on: December 23, 2002, 12:04:00 PM »
but swim ran a 3g MeNH2/al/hg Osmium style yielding 2g of the hcl salt, 52%. not quite sure what's holding back the yields, maybe he balled the extra heavy duty foil too tight and dripped in all the ketone over 1h while not enough Al was exposed. it took all night for the foil to finish breaking down.

then swim ran a 4.1g MM reduction. timed it very nicely, 1h of ketone drip and 15 minutes later the Al was gone. basified with 43.3g NaOH in 50% aqueous solution. pH went up to 14 and sludge turned black (argh). 10% yield.
previous 1.6g MM reduction gave 41% yield, nothing special there.

so swim got some flashing, amalgamated 12.75g in 50ml MeOH, dripped in 96g of 15% nitro (14.4g MeNO2, about 77ml MeOH, some castor oil, no water added), let reflux 2h, added 15.7ml 50% NaOH, let reflux and stirred overnight. swim boiled it over trying to distil out of a flask 4/5 full (please, laugh...), switched to a bigger flask, and distilled 60ml of 4.6% MeNH2. sludge didn't swell up during gentle distillation.

so, abacus (love your synth, i really do) reduces 3mol of nitro and gets 1400ml of 6% MeNH2 ~= 2.2mol (disregarding the density of MeNH2 ), 73% yield. swim may have alot to learn, but at least he knows to add more MeNH2 than this to 178g of ketone... for 2.2mol MeNH2 use 130-156g ketone. pm me for details.
anyway, swim reduces .236mol nitro (undistilled 15%) and gets .0725mol, 31% yield.

so basically, swim recovered half the MeOH added origionally and got half the yield expected. any suggestions? add more MeOH to the sludge and distil again? use distilled 8% MeNO2 (doubling the solvent volume) next time? its probably the fukkin castor oil... bad shortcut.

anyway, closer to the origional topic, how do you gas 100+ grams of amine? it seems to me that dripping hydrochloric onto sulfuric, the sulfuric is going to get diluted and useless before enough gas is put out. so who prefers NaCl + sulfuric for gassing alot of product? or do you add pregassed IPA, then crash the salt with acetone (or ether)? last is probably the most idiot-proof large scale option if you weigh the IPA, determine HCl concentration, and add an exactly equimolar amount.

Osmium

  • Guest
> so basically, swim recovered half the MeOH ...
« Reply #79 on: December 23, 2002, 01:24:00 PM »
> so basically, swim recovered half the MeOH added origionally
> and got half the yield expected. any suggestions?

Do it at a bigger scale.

> anyway, closer to the origional topic, how do you gas 100+ grams
> of amine? it seems to me that dripping hydrochloric onto sulfuric,
> the sulfuric is going to get diluted and useless before enough gas
> is put out.

One solution to this problem is using more H2SO4. A gas generator suited to generate enough HCl gas for 10g freebase will most likely not cut it when you want to gas 300g with it.
Isn't that kinda obvious?

I'm not fat just horizontally disproportionate.