Author Topic: Processing 1 Mole Ketone Using Nitromethane  (Read 4112 times)

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hCiLdOdUeDn

  • Guest
Any moron who can follow simple directions should ...
« Reply #40 on: December 03, 2002, 01:13:00 AM »
Any moron who can follow simple directions should be able to make methylamine from paraformaldehyde & ammonium chloride by the kilo in half a day.

I dont own large glassware so I have no reason to make that much! :)  Besides, abacus method of making methylamine in methanol is great. ;)

Have a GOOD day!!  :)  ;)

Sink or SWIM

abacus

  • Guest
Indeed
« Reply #41 on: December 03, 2002, 01:34:00 PM »
It took me 5 days just to make 1/2 kilo methylamine.hcl using hexamine/HCl and formaldehyde/am.cl.

Using the same size glassware I can be finished processing 900g ketone in 5 days with nitro as I outlined.

DON'T use foil for the nitro reduction, you must use thick aluminium as GOD found out.  Also a bit more 50% NaOH may help.

Finally, keeping the oil bath temperature below 210DegC when distilling the freebase eliminates the problem of charing the freebase and has increased yields with only about 5% being lost when distilling as Osmium suggested.

Thanks to all

Abacus

raffike

  • Guest
200 grams of methylamine in 2 liter flask in one ...
« Reply #42 on: December 03, 2002, 04:14:00 PM »
200 grams of methylamine in 2 liter flask in one day is piece of cake.I also have 10 liter flasks,so 1 kg/day is more than i could use next day.

For those about to synth,we salute you

hCiLdOdUeDn

  • Guest
Lucky you, I own 19/22 glass joint sizes with my ...
« Reply #43 on: December 03, 2002, 10:41:00 PM »
Lucky you,

I own 19/22 glass joint sizes with my largest flask of 500mL. The 19/22 joint sizes works well for distilling ketone without loss of much product.

Also abacus,
Why would one want to add NaOH to post nitromethane reduction? Wouldnt this release the methylamine gas and cause it to come out of the methanol? I would want as much methylamine gas when distilling over in my methanol as possible. I understand the point of basifying when reducing ketone but why post-nitro reduction?



Sink or SWIM

GOD

  • Guest
ok- swim switched to Al flashing thats about half ...
« Reply #44 on: December 03, 2002, 10:49:00 PM »
ok- swim switched to Al flashing thats about half as thick as Abacus' reccomendation.  MUCH gentler rxn...  400mm condensor took care of things just fine, plus a vigreux with cold assed air beeing fanned from an open window. 

Of course, now there is a new set of problems/questions  ::)  :-[

-first off, swim forgot to take into account that there would bee more surface area considering the fact that his Al is half as thick.  He used the same ratio of HgCl2 as called for.  He added Al, dumped in his Hg salt, then added the methanol.  While that was sitting, he measured out his nitro/DH2O and also separated the initial part of that mix from the addition funnel.  He took his time (10-15 minutes), looked down at the flask and saw that the Al had dulled, and there where little bubbles coming up.  He figured all was well, so he started the rxn.  He noticed that it appeared as if only one side of the Al amalgamated- when peices where floating around, one side would bee brown-near black, and the other side would bee shiney Al.  This was pretty consistant with almost every peice that he saw (some had little blotches on the shiney side) -is this because swim shoulda waited a little longer to start his addition, or is it a sighn that his flashing may not bee the right stuff? (sorry, this is a newbee question, but I have one or two more related to this procedure)

-Swim noticed that unlike when he used foil in the past, everything seemed to settle on the bottom more (all the crap) whereas with the foil, he would often find that the crud seemed to float.  He had left stirring on for the greater part of the rxn figuring he didnt want to hand swirl so much seeing as how he didnt know how vigarous of a rxn to expect.  When he did swirl, he saw quite a bit of unreacted Al on the bottom (lots o shiney stuff even past an hour into the rxn, MUCH more unreacted stuff than what he was used to with foil).  He also noticed that even as the floating peices that appeared to bee near used up moved around, they seemed to remain in tact, and it was as if the flashing had retained its shape, but grown in thickness from the dark side, and it looked like its shape was beeing held together by the shiney, unreacted side(s) of the square -once again, is this normal, or is it an indication that there might bee some kind of coating on the flashing? 

-Last question, upon addition (swim did it slowly with his addition funnel) of NaOH solution, what kind of color changes (if any) are expected to occur?  Swims solution turned a lighter shade of grey with light green-tan swirlies in it to a darker tan-green-grey to a dark, brownish color.

Im not the bearded man upstairs, Im a bald guy with a healthy penis. So open yer pie-hole!

hCiLdOdUeDn

  • Guest
When swim did an al/hg nitromethane reduction 572 ...
« Reply #45 on: December 03, 2002, 10:59:00 PM »
When swim did an al/hg nitromethane reduction 572 years ago,with Hg2I2 (tincture of iodine). His aluminium did not change colors (he used thick aluminium pie pans). After addition of tincture 45minutes it started to bubble and a grey sludge formed on the bottom. The solution was cloudy and grey and that is when he slowly poured in nitromethane. After the reaction finished he added 600mL of 25% NaOH and a strong fish/ammonical smell was released and things started to get nasty. The solution started to boil and then it calmed down. The post-al/hg was a light brownish, he used RC fuel, and some dark sludge was on the bottom.

It seems to me, GOD, that it worked out for you! Using thicker aluminum is good! Aluminum foil is probably better for ketone reduction with methylamine as it isnt as exothermic.

Sink or SWIM

scram

  • Guest
I had similar problems using pie tins once.
« Reply #46 on: December 03, 2002, 11:34:00 PM »
I had similar problems using pie tins once. Even after 50 minutes the metal was still shiny. I don't remember if it had dark spots on it but that does sound vaguely familiar. Im waiting to watch other have more success as I see many of us are switching to flashing/pie tins before I try my luck again with it. My post reaction mix after NaOH addition is either dark grey or after a 12+ hour reaction black.

Osmium

  • Guest
> It seems to me, GOD, that it worked out for ...
« Reply #47 on: December 03, 2002, 11:35:00 PM »
> It seems to me, GOD, that it worked out for you! Using thicker aluminum is good!

Goddammit! Of course it is good!!!
Why do you think I'm fucking preaching to use thick Al for 5 fucking years?!? There's no need to reinvent the wheel!
And when did it become fashionable to skip using the search engine or reading Rhodium's site?

Fuck this, just go on everyone fucking up the signal/noise ratio a little more.

I'm not fat just horizontally disproportionate.

abacus

  • Guest
Come on people, think about it
« Reply #48 on: December 03, 2002, 11:59:00 PM »
Why don't you go back and read what I wrote, then read osmium al/hg on Rhodiums site, UTSE to read what Osmium wrote about the al/hg.  Its all there.

I repeat, alumimium sheet EQUAL or GREATER than 0.3mm thick.  The sheet chem suppliers sell is 0.6mm thick so thick is good for very exothermic reactions such as with nitromethane.

Then use your favorite foil for the ketone if you like.

Some pie tins etc seem to be alloys which don't work that well.  Try and get soft uncoated aluminium flashing, then test it with a little hgcl and nitro first. 

ALso, there is some leftover aluminium after the reaction, so feel free to use less.

I used 50% NaOH for a reason, which was to help break up the sludge without adding too much water, to help finish (speed up) the reduction of any left over nitro, and to help drive out the methylamine gas when distilling.  I said that at the beginning damn it!  And yes, the sludge turns brown.

Feel free to try it without any NaOH, I just never got around to trying to distill out the methanol/methylamine without it. 

Thats all I'm going to say, the improvements can be someone else's problem.

Abacus   

hCiLdOdUeDn

  • Guest
Thanks! Have a HAPPY day ;-) :-)
« Reply #49 on: December 04, 2002, 12:15:00 AM »
Thanks!

Have a HAPPY day ;)  :)

Sink or SWIM

Bubbleplate

  • Guest
If Only One Side of the Al reacted
« Reply #50 on: December 04, 2002, 03:22:00 PM »
Sounds like it had some sort of coating on it, plastic or similar. Some flashing is treated that way so it doesn't weather so fast when exposed to the elements.
Take a piece of your Al, and scrub BOTH sides with steel wool then throw into some Hg solution and see what happens. That should confirm if the Al is coated.

lab_bitch

  • Guest
Watch What You Post
« Reply #51 on: December 05, 2002, 08:54:00 AM »
Broadcasting to the DEA that you regularly produce kilos of MDMA is not a very safe practice.  You should assume that the DEA has read this and knows your I.P. address.  If this address happens to be linked to a connection under your name (in other words, you access the hive from your home computer) you can assume that they know who you are and where you live.  It's amazes me, the stuff that some people say around here.  If I were producing anywhere near that large of an amount, I wouldn't even log onto the hive unless it was from a remote location (i.e. - the library).  I'm not trying to put you down or anything; just don't want anyone to become another victim of Uncle Sam.

Protium

  • Guest
In my own defense
« Reply #52 on: December 05, 2002, 09:56:00 AM »
I'm not producing anywhere near that amount. ;D  :P

Pr(+)tium

BlingBling

  • Guest
Im retired!
« Reply #53 on: December 05, 2002, 10:50:00 AM »
Im protected by the retired bee act of 2002.  :P

hCiLdOdUeDn

  • Guest
Remember! No one actually makes this "stuff" its ...
« Reply #54 on: December 05, 2002, 06:44:00 PM »
Remember!

No one actually makes this "stuff" its all talk. ;)

Sink or SWIM

lab_bitch

  • Guest
Re: EDit: But I think the "kilos" i purchase may ...
« Reply #55 on: December 06, 2002, 07:43:00 AM »

EDit:  But I think the "kilos" i purchase may be a bit big coz I end up with 1050mls Isosafrole from them and after checking notes I got 550g MDMA.HCL from the last one after vacuum distillation of freebase, gassing in acetone AND recrystalling (twice) in ethanol.




This is the specific example I was talking about.  If I were a DEA agent, he would be under constant surveilance.  Never underestimate an agency that recieves billions of dollars a year to do shit like this.  Your best chance of not getting caught is to not let them know you exist and assume that every word you speak is being recorded at their headquarters.  If they can intercept the communications of those terrosist bastards, they can intercept your's as well if they are looking for someone who does what you do.

Also, it doesn't matter what kind of code words or evasive phasing you use.  When someone writes "SWIM just cooked up a successful batch of 1 kg of product" the DEA knows that 9 times out of 10, the word "SWIM" can be replaced by "I".  If they even suspect that you are doing something like this, they will enter your name into their list of people to get fucked.  Remember - they don't have to play by the rules if no body finds out.  Although they can't use an illegal wiretap as evidence, they can still gather information from it.  Eventually, they'll have enough information to intercept you while you are actually performing some illegal activity (i.e. - transporting) that would grant them a search warrant.  It's all over from there.


abacus

  • Guest
Hives security
« Reply #56 on: December 06, 2002, 07:47:00 AM »
Yeah but, doesn't the DEA need the help of the hives ISP which I understand it won't get.

Also, SWIM's access to and connection with the hypothetical lab has finished, so no problem.

Abacus

lab_bitch

  • Guest
They might not be able to get the IP from this ...
« Reply #57 on: December 06, 2002, 02:12:00 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.  Besides, how do you know that the Hive wasn't set up by the DEA and Rhodium is really Asa Hutchinson himself?  I hope not, but the feds set up sting operations in a similar manner.

abacus

  • Guest
Get a life
« Reply #58 on: December 06, 2002, 03:55:00 PM »
Lab bitch

I live in Asia, how the fuck is the DEA going to get my IP address without the help of the hives ISP and how the fuck are they going to find my ISP router.  Do you think the US will invade Asia to find it?. 

Stop shooting up that meth and get a fucking grip.

Abacus


Barium

  • Guest
As long as you follow your countrys laws the DEA ...
« Reply #59 on: December 06, 2002, 05:07:00 PM »
As long as you follow your countrys laws the DEA cannot do jack shit. The US in general, and the DEA in particular, has a hard time realizing thir laws aren´t applicable worldwide yet. As long as you follow your laws, and your government isn´t too quick bending over to the DEA cocks, you should be alright.

Catalytic hydrogenation freak