Author Topic: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg  (Read 6095 times)

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weasil

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Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #40 on: April 11, 2001, 07:28:00 AM »
I swear all the guidelines have been followed though which really beats me...I'm mystified!
When did failure finally become success though? Did it take switching chemicals to something a little less over-the-counter or did you need to carefully revise you’re practical methods? Now that you are competent you can churn out the crystals what tips do you have for newbees? Does the initial investment repay itself or is that a debt that cannot be recovered? I know these questions will yield different answers from different bees but nearly all bees have failed on their first attempt regardless of their prep work. In foundation organic lab I follow the course handbook and I nearly always get crystals despite not doing nearly as much research into the synth as have done in the hive. This is what makes matters puzzling. Have not a clue where went wrong. If photoshit so crap why is it recommended?
This time post amalgation still orange (4th time). This time difference is it smells of ammonia!

weasil

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #41 on: April 11, 2001, 08:38:00 AM »
Toluene extracted goodies from the mixture. During 1st water wash white crystals ppt in water layer thst float upwards into lower tolly layer. Think eh? Tolly still orangy. Must get to the bottom of this.
And did. Nothing but junk. Only crystals that have been formed here are NaCl.

hypo

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #42 on: April 11, 2001, 09:22:00 AM »
I'm not sure i understand what u are saying here.

The crystals you are talking about fell out after gasing or after washing?

weasil

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #43 on: April 11, 2001, 10:09:00 AM »
Yes, I don't understand this either. To be honest...I don't think anyone does [this is where you have a laugh at my expense]. Crystals ppt out during water wsa hof orange toluene. Water is yellow coloured? Guess this must have something to do with impurities.

hypo

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #44 on: April 11, 2001, 10:23:00 AM »
Yes, this will stop when you start using pure ketone. Just throw away any precipitate during washing! It may contain Hg! Go on with the washes (some water, 1 or 2 conc NaCl). The toluene layer will never get colorless. Gas. If there are crystals, they will be red. Wash with lots of acetone or recrystalise with IPA/Acetone to get snow white crystals.

DiethylEtherMan

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #45 on: April 13, 2001, 11:28:00 PM »
Excuse me, bro...Mr. Hydro, but the toulene certainly does get colorless, on my world, at least. Clear as the clearest water I have ever seen as a matter of fact.

Anyway, thats just in my experience.

You need an oil change. But, your car will probably die before you give it one.


If some of us were not so far ahead, the rest of you would not be so far behind!

hypo

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #46 on: April 14, 2001, 03:55:00 AM »
Yes, in my world it will get clear too, given that you start out with reasonably pure ketone. Actually it will be pretty clear from the start.

IMO weasil is using dirty ketone and gets lots of organic shit. You cant wash that out with water. Still, there should be lots of good stuff in the toluene layer (if he did use ketone at all), the Al/Hg is pretty forgiving...

weasil: try dissolving the ketone in DCM, wash multiple times with water and Na2CO3 solution and distill again. Check the temperature.

terbium

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Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #47 on: April 14, 2001, 09:32:00 AM »

(if he did use ketone at all)


Yes, often, when I see people complaining that their amination/gassing didn't produce any product, I wonder if they even had any ketone to start with. This is why I recommend the bisulphite test to verify that you possibly have a ketone.

Some people say; why bother with bisulfite, just aminate but bisulfite is easier than Al/Hg/Nitro especially for people who are working in a back room with almost no equipment or experience.


weasil

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #48 on: April 14, 2001, 11:12:00 AM »
I can't understand why no ketone => good PdCl2 + Benzo and Safrole were used. MM's synth was followed to the key with the only modifications being the ommitting of the filtering and the first two sets of washes. Yeah, in hindsite should'nt have taken shortcuts. Collected fraction 20C+ what safrole came over at. Use of vigrex was necessary though so could'nt collect richest part of the fraction. So yeah impure ketone maybe, but is a bit of safrole enough to completely fuck things up this bad?

ACcidently added entire impure ketone to baking soda for bisuphite addn (have to run up and down three flights of stairs so shit just happens nomatter what). Will continue to do test and see what happens.

Dumped that ketone and am now phyched up to do a third batch overnight and am now distilling the last of my sassafras. OKay am pissed off about wasting hundreds in chems and hours of time but that is life. Am gonna follow MM with no compromises. I can do this shit without any paper infront of me I know it so well. Weasil is gonna die once he finds success.

baalchemist

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Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #49 on: April 14, 2001, 02:02:00 PM »
Over the years many bees have had the same problem with the wacker,theres no guarantee that it will produce ketone for reasons unknown. Toluene layer in these parts is always clear/colorless. If there is color(green/yellow), then an A/B is absolutely necessary to avoid the red oil BS(which is ketone/hcl mutant). After all your Al reacts, look at reactions overall color, if you see green/yellow toss some more Al in. This may help in some instances,but not all, again ketone purity plays a big part along with addition timing.

weasil

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #50 on: April 14, 2001, 02:46:00 PM »
Weird, aint it? How some people can have success first time even with sloppy procedure, while others can do the reaction with the upmost care and fail. I would say this is something unique to clandestine chemistry and blame it on the chemicals themselves. Believe me I know all about acetone competing side reactions and the like so I am careful like one should be. Now this time will be attempting this at this level. If it does'nt work there will be no alternative than to buy from alternative sources.

spric

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #51 on: April 14, 2001, 06:15:00 PM »
Just a note if you want to mess with some sodium bisulfite,  Any spa or pool place will sell you a pound or two of pH/alkalinity decreaser for a few bucks, which is 94% sodium bisulfite.  REal easy way to get the qualitative yes or no.  I think it is impossible to screw up an amalgamation with clean reagents.  Shitty, shit shitty runs  should still give you a few grams vitamin E.  It will work one day, just wait, and you will get very excited, like a 5 year old kid on christmas eve.


good shit will blow the jam out your toes and make your boogers go south for the winter.

terbium

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #52 on: April 14, 2001, 06:23:00 PM »

Any spa or pool place will sell you a pound or two of pH/alkalinity decreaser for a few bucks, which is 94% sodium bisulfite


Really? I would have guessed that it would be much more likely to be bisulfate than bisulfite.


spric

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-
« Reply #53 on: April 16, 2001, 08:50:00 PM »
oops, you know what I meant


good shit will blow the jam out your toes and make your boogers go south for the winter.

weasil

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #54 on: April 17, 2001, 05:02:00 AM »
Well the first batch of ketone was extremly pale yellow when using photograde PdCl2. For this batch 3 washes with NaOH (10%) is recommended. Don't even bother filtering. I hate taking a long time on this because surely the ketone would decompose if one were to heat this for a prolonged amount of time. Hell, I even feel the need for a rotovapp olready. My 2nd hand Leybold Divac is certainly capable of doing it's job and is well respected compared to some of the junk sold at auctions. Check the blue tone in the Nasa. Someone I don't know said they got a lighter tone with the same colour on their 2nd run after discarding the forerun ~20mls prior to the fraction that was collected 20C+ the temp of the safrole.

Osmium

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #55 on: April 18, 2001, 06:20:00 AM »
Well in my opinion that colour is definitely yellow, even when distilled twice with vigreux columns.
I never experienced any other colour than that.

DiethylEtherMan

  • Guest
Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #56 on: April 18, 2001, 02:56:00 PM »
Tone, in its purest form, is certainly yellow. Although, in my mothers house, after watching her do benzo after benzo, I have seen colors ranging from yellow, to yellow with green undertones, and to a forest green color, which is the most recent. And this tone has worked absolutely fine with no problems.


If some of us were not so far ahead, the rest of you would not be so far behind!

dr_gonzo2

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Re: MM writeups of MeOH benzo wacker and MeNO2-Al-Hg
« Reply #57 on: April 30, 2001, 01:14:00 PM »
Hi everyone, this is Dr Gonzo, I am making one of my twice-yearly appearances and after this post I'm afraid I have to go away again.

I have a couple updates regarding Methyl Man's amalgam and my photo essay that appears on Rhodium's page.  First, as my client got better with this technique (and double-distilled the ketone), he brought his yields up to 21.0 g of the hydrochloride from 25.0 g of ketone.  He maintains his opinion that for the MDMA-producing hobbyist (as opposed to the professional cook) the slightly less-than-perfect yield of the nitromethane Al/Hg is easily offset by the simplicity of the reaction, the unwatched reagents needed, and the good chance of success.

Also, my client asked a friend to do an NMR of some MDMA HCl he had produced with this method.  The workup for this batch was a xylene extraction from the reaction mixture, double bicarbonate wash, double NaCl wash, double water wash, dry the approx. 800 mL xylene extraction with MgSO4, then carefully gas, filtering out precipitated crystals often and continuing to gas.  Then a final xylene wash of the filtered crystals.  Friend was extremely impressed with the purity and estimated it at being 99.5% or better.  Any impurities were tiny, tiny peaks on the NMR spectrum, almost not there at all.

I'll probably email Rhodium and ask him to update the essay, and I'll see if I can get the NMR spectrum added too.  Keep up the great work, everyone!