Author Topic: Al Amalgam Rate  (Read 965 times)

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Sir_Seretone

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Al Amalgam Rate
« on: August 10, 2003, 05:20:00 AM »
Followed Brisgtsar right up and Ketone looks good. Followed the MM NitroMethane Amalgam and couldnt get the rate quite right and in the end had 10 grmas of Aluminium left over after reaction was complete. I as thinking I might get a poor yeild but a yeild none the less. Procedded to Gas after a minute nothing then the solution went a cloudy white for a few seconds and then turned a light brown. What is this brown stuff .. and is it possibile that no yeild is a result of a poor amalgam rate and the left over ALuminum is a good indicator I fucked up ?


OcoteaCymbarum

  • Guest
Follow this exactly
« Reply #1 on: August 10, 2003, 09:15:00 AM »
And you will get MDMA everytime.

750 ml MeOH
150mg HgCL2(eyeball it)
27.5 g Aluminium foil, properly nuggetized. You might have a little left at the end, but not 10 grams.

I like to add about 5 ml of water to that mix(my MeOH is anhydrous). Also, I like to add a bit of nitromethane to the mix prior to drpping in the ketone/MeNO2 mix. Maybe 2-5 ml.

Drip in your ketone/MeNo2/MeOH. Addition should take about 30-40 minutes after your aluminium just started to float(which signals to start the addition)

Have a long condenser, more then 200mm.

Leave to stir for 3 hours. Add your NaOh solution and extract with your non-polar.

You now have your freebase in np.
Now you need to clean it up. MM doesnt clean it up enough to me. A minimum is an A/B to get quite pure MDMA.
Distilling after would be best.

So wash your Np with 5% NaOH a couple of times to get rid of any water soluble impurities present.

Then Acid extraction. Use 10 % HCl, 100ml then 50 ml extractions. At that scale, all the MDMA salt goes into the first 100 ml, but do another extraction to be sure.

You now have you MDMA in water. Wash that solution with fresh and clean non-polar. This is to get rid of np soluble impurities.

Basify your water solution until MDMA is turned into freebase again. The pka for MDMA is 9.6 which means that bringing the pH to 12 is well enough.

Extract that basic water with a non-polar to extract the freebase again.

You've now completed an A/B.

Dry the np and gas. You will get white crystals.

You really have to clean up your freebase or else it will turn either yellow, brown, maybe even red.

This is hard to fuck up. You wont maybe get 20 grams yield the first time, but after a little practice, youll get there.

For a proper answer, you will need to provide more details as to what you've done, how it looked, etc. This is where keeping track of everything you do, especially when you start, is useful. Keep a lab book. The only problem is the extra proof it gives to the DA. Good luck and dont give up you're so close!

rudebwoy

  • Guest
?
« Reply #2 on: August 10, 2003, 12:39:00 PM »
I don't think you answered his question on drip rate.

Just do 3-4 rxns and you'll get the hang of it.

Just hunch over in front of your rxn vessel like the hunchback of notre dame and then use your proper judgement from what you've read on the hive.

My contribution is,
when i used to dream up the nitro solution, I figured out a good way of finding how fast the rxn is going was just by watchin the speed of methanol condensing from the condenser.  Then I just matched it sorta with the stopcock.
Just use your instinct.

As for the brown oil falling out, your np layer wasn't dried or the gas wasn't dried.
just redo the a/b and u'll get it.

Happy cookin.


hypo

  • Guest
brown crap
« Reply #3 on: August 10, 2003, 12:52:00 PM »
> What is this brown stuff ..

this is what you get, when you don't a/b and don't distill.
yep, there's colored crap coming through a/b, so distilling
is more or less a must. when you have good yields, the colored
crap only comes after second or more gassing, but when youe
yield is low and your toluene is not anhydrous, it happens,
that it comes with the first fraction.

put your toluene in freezer and filter of the crap/product mixture.
if you have enough of brown crap, you might try to boil in a little
bit of acetone, cool and filter. should give white crystalls.

an alternative to distillation (which is easier than ketone distillation,
so _no_ excuses!) is to do a real a/b and to gas from acetone, since
acetone seems to dissolve the crap, but not the good stuff.

> in the end had 10 grmas of Aluminium left over after reaction was complete.

strange, i've never seen the MeNO2/Al/Hg not work. usually the reaction with
MeNO2 is so violent, that it tears even 0.3mm sheet apart. where does the 10g
figure come from? did the reaction go (very) hot?

Sir_Seretone

  • Guest
Aluminum
« Reply #4 on: August 13, 2003, 09:47:00 AM »
The Aluminum was .6mm thick and obviously after that reaction at least .3 mm too thick. Wil try and find some heavy duty foil and use that next time.

wyndowlicker

  • Guest
Hey now,
« Reply #5 on: August 13, 2003, 06:45:00 PM »
Hey now,


 Im still trying to figure out where you can buy pre-nuggetized al foil. ;D Ive reduced my al foil to 26g per MM write-up instead of the 27.5g It pretty much cleared up the problem.Also are you allowing you tone to reach RT before you start your addition?Im almost sure your yields go down when your tone is ice cold.Add 4ml nitro before your addition has begun.It will start to get quite hot in just a few minutes.Then begin.This reduces the loss tone.And please gas your crystals out slow enought to not over gas, it will happen if your not careful ,changing your product color pretty quickly. :P


abolt

  • Guest
???
« Reply #6 on: August 14, 2003, 06:51:00 AM »
Im almost sure your yields go down when your tone is ice cold

Why would you assume this?

Also, what are your yields via this route?


Rhodium

  • Guest
cold ketone
« Reply #7 on: August 14, 2003, 12:34:00 PM »
Ice-cold ketone would form the imine very slowly, but could still be reduced to the alcohol by the Al/Hg. But of course, it will on the other hand be rapidly heated by the warm solvents, so I don't know if it has any practical significance...

slick14

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What type of aluminum does swiy use.
« Reply #8 on: August 27, 2003, 07:58:00 PM »
What type of aluminum does swiy use. Swim has had similar problems using aluminum oven bags which used thicker al.


baalchemist

  • Guest
Over the past 5 years, Baal has never had to...
« Reply #9 on: August 29, 2003, 06:23:00 AM »
Over the past 5 years, Baal has never had to distill the end reaction mix not once & gets a water-clear toluene extraction everytime. End weight after gassing is equal to & sometimes more than the amount of ketone that was started with. On a small reaction of 27.5g's, the addition rate should be more like 15-20 minutes tops. The 30 min. addition mark is where yields start diminishing quickly. If there is still aluminum unreacted, keep it running longer and put some heat on that bitch til its all consumed properly. Some catalytic types of reactions need that extra heat-energy to keep it up to speed with the rest of what is going on in the pot. Pre-loading the reaction with nitro has no effect whatsoever, silly superstitious crapola. There is already an excess in the ketone/nitro/meoh mixture that gets dripped in, and that is what ultimately is driving the reaction to its proper formation. Practice & solid observation skills prevail in getting the excellent yields.........


abolt

  • Guest
The 30 min. addition mark is where yields...
« Reply #10 on: August 29, 2003, 08:43:00 AM »
The 30 min. addition mark is where yields start diminishing quickly.

Why do you think this happens Baal? f

From the loss of agitation, due to the reflux slowing down?

Loss of Methylamine, due to the reaction going hard?

Why does this happen?


raffike

  • Guest
Raf thinks it might because of Al being gone...
« Reply #11 on: August 29, 2003, 09:02:00 AM »
Raf thinks it might because of Al being gone before all ketone reacted.Raf tests this drip-in-ketone-over-some-time with methylamine.He just got some good ketone to play with.Should give higher yields.Mix alcohol,aluminium,methylamine/NaOH solution in a rb flask,add HgCl2 and wait till temp starts to rise,drip in ketone and keep temp around 50-60C.Will post results


abolt

  • Guest
Raff
« Reply #12 on: August 29, 2003, 09:18:00 AM »
I'm pretty sure that Baal is talking about Nitro.

I just can't understand his remarks about yield diminishing after 30 mins.

The Methylamine can't just dissappear, if the condensing is any good.

I believe it is due to the agitation in Baal's "fast addition" reactions slowing down. Thereby slowing down the reaction at the activated aluminium interface, or it could indeed be that the Aluminium Baal uses is so thin that it burns up inside 30 mins.

If this is the case then good stirring, or thicker Al, would take this "Diminishment of yield" point past 30 mins.


raffike

  • Guest
Baal uses nitro,yes,but adding ketone dropwise
« Reply #13 on: August 29, 2003, 06:48:00 PM »
Baal uses nitro,yes,but adding ketone dropwise should give higher yields than adding it all at once.Not sure but raf will run a test.