dream turned nightmare

[krazy89]

Hey everyone,

My al/hg dream turned into a gummy nightmare! i don't know what went wrong?  here's what happened:

did MM al/hg and everything went pretty smoothly, with end sludge that is light gray w/ a little bit of blue.  left the sludge refluxing and stirred for about 16hrs after addition.

after, workup was as MM: add 35% NaOH, extract with 400ml/150ml/100ml xylene, then washes: 3 dH2O, 1 NaCl

QUESTION: what color should the xylene extractions be? mine came out light purple!?!?!? (after H2O wash, took out the purple and left a very pale yellow color)

dried with about 35g MgSO4, filtered then put in the fridge

set-up for gassing: muriatic into H2SO4, gassed for about 2-3 mins and nothing, kept going and xylene got really cloudy (but didn't see any crystals) so kept gassing, then this brown gummy goo formed on in the xylene.  total gassing time was maybe about 15-20 mins.  stopped gassing.

now i have this brown goo and the xylene got a lot darker in color too.

took out the xylene, washed with 2x dH2O, 1 saturated baking soda, 1 saturated NaCl

after, xylene was a very pale yellow color but it wasn't clear, it didn't let much light thru it at all.

i've read that what happened was overgassing.  Can anyone help me out here?  second dream is about to come and need to know if the old xylene is salvagable or just start again!?!?

KraZy89

[DoctorFeelgood]

is not my prefered method, but i have done a few batches a few years ago. consider making methylamine first e.g. from hexamine - very easy. then consider aminating with the 'wet nabh4' method or with osmiums al/hg with meam. 
did you scale it down or up or did you do it like in the writeup? did you check your alufoil? If not, just put some aluchips in a 250ml rbf, add some meoh/hgcl2 and let it aminate. after addition of a few ml of nitro, a noticeable exothermic reaction should be the result. if not, the alu is useless. In my experience, the steelblue color is not a true sign for a successful reaction.
The Toluene/Xylene phase (on top) should be clear, maybe with a little bit of sludge between the two phases (this depends on how carefully you did the separation before).
i never had a purple colored xylene/toluene, but a little bit yellowish sounds good to me.
brown goo sounds not very good. check the ph of the xylene, if it is acidic, there should be no (more) base in it. did you gas just with h2so4 and hcl? in my case this did not work, i prefered the nacl/hcl + h2so4 method or the cacl2 gasing method.
i never had a problem with overgasing of xylene/toluene/base. it could occur at the end, e.g. after gasing it 2-3 times. normally the xylene/toluene turns into a coconutlike solution, which is very thick, full of snowwhite xtc, which should be recrystalized e.g in isopropanole (IPA).
In my mind, MM is cleaning far too less. consider doing an A/B and of course vacuum distill the freebase, which is very easy (bp = a little bit higher than mdp2p). you will be left with a redish tar (higherboiling impurities, sure not edible...) and a waterwhite mdma freebase, which will kick you out of your pants. the high/turn is noticeable better if you do it this way !!!
I'm sorry, this is all i remember about this.
greetings

[DoctorFeelgood]

your xylene starts to get cloudy. this is normal, this are the crystals. if there is too less mdma in it, then it is not getting thick & coconutlike. it seems, that your al/hg failed, maybe there was too less meam present. what you will get first, is a snowwhite powder (after drying), to get real crystals, you have to recrystallize it slowly (then the crystals look like big-grainded sugar)...

[abolt]

what color should the xylene extractions be? mine came out light purple!?!?!?

Never judge a reaction by it's colors.

kept going and xylene got really cloudy (but didn't see any crystals) so kept gassing, then this brown gummy goo formed on in the xylene.

This is because your product is not properly cleaned. Yoou should do at least, a full A/B cleanup of your amine before gassing. UTFSE to read up on A/B washes.

If you expect decent answers, you should give decent info.

Was your ketone tested?
Was it properly distilled?

now i have this brown goo and the xylene got a lot darker in color too.

took out the xylene, washed with 2x dH2O, 1 saturated baking soda, 1 saturated NaCl

You washed the Xylene again, after gassing? If you did then most of your product is most likely in your washes.

i've read that what happened was overgassing.

The chief has stated that "overgassing" is a fallacy, I agree. The brown shit you had most likely had some amine in it, that was very dirty due to the fact that you didn't purify it properly. Hence, the brown color. 

Can anyone help me out here?  second dream is about to come and need to know if the old xylene is salvagable or just start again!?!?

If you washed again after gassing then the product would be in the first of your "2 x DH2O washes".

Evaporate the water, dissolve the left over sludge/crystals with strong NaOH solution, extract with fresh xylene,  wash 3 times with 5% NaOH and discard washes.

Then make acidic with 10% HCl, tap off the lower water layer and place the xylene aside. Now wash the acidic water with 3 x equal volumes of fresh xylene and discard or recyle xylene washes.

Now you can either:

1. Make basic again with strong NaOH solution, extract with Xylene, dry with MgSo4 and gas.

Or better yet:

2. Make basic again with strong NaOH solution, extract with Xylene, distill away the xylene and then distill the freebase, place distilled freebase in fresh xylene, dry and gas.

The very best advice I could give you is that you need to do a lot more reading before commencing again.

.........or you will keep having nightmares

[krazy89]

hey guys....

as for more info, i didn't test the ketone as it seem to have all the right properties of ketone: color was clear yellow, and the temp that it came over was about 140C which is about right.

as for the al/hg reaction, i did it exactly like MM's writeup and followed the washes and extractions according to him.

I have a question about MM's al/hg workup:

after the reaction, washes, extractions, i should have about 500ml of xylene/mdma oil.  from here, should i just gas that? or should i distill it? and if i distill it, what fractions will be coming over? and what should i do after?

thx for all the help.. i'm a real noob  

KraZy

[DoctorFeelgood]

after the reaction, washes, extractions, i should have about 500ml of xylene/mdma oil.  from here, should i just gas that? or should i distill it? and if i distill it, what fractions will be coming over? and what should i do after?

no, do a standard A/B first (short description):
starting with mdma in xylene, allready washed.
prepare about 200ml 5-10% HCL solution and enough 10% NaOH to neutralize it later.
put xylene in a sepfunnel and add 150ml HCL and shake. the mdma goes into the hcl as an salt. separate the hcl and repeat with 50ml hcl. save xylene for further use, e.g. you can distill it to clean it up. combine hcl separations and pour into cleaned sepfunnel.
slowly add the cooled NaOH solution to your sepfunnel, until you see the raw base (brownish color) falling out to the bottom of your sepfunnel. check PH, when >11, no more base will fall out. separate the raw base into a beaker or whatever you want. add 200ml DCM and shake. the mdma should be now in your DCM.
separate the dcm from the rest and setup for distillation, distill dcm off (bp 40 C) and vacuum distill the rest (in my case about 155 C) to get very pure waterwhite mdma base, which you can now dissolve in xylene. THEN gas it.

greetings

[krazy89]

thx doctor for the help...

as for after the a/b washes... when i get the white mdma oil, can i just use BS method of adding hcl and acetone and then distill til the cystals crystillize in the flask?

KraZy