Finally work done with complet succes!!
.
I think maybe my experience can help others that want to try that reaction.Maybe exists more high yielding methods to mda from mdp2p,but this method it´s so easy and the yields are just good enough to put that reaction as a one of the best to mda from ketone if one have access to cyanoborohydride.
I was reading a lot about cyanoborohydride,reading a lot how that reaction works better on big batches than small ones,how Ph can fuck the cyanoborohydride activity(may stay betwwen 6-8),reading a lot about best reaction time to get maximum yields(36 hours),reading s lot about nasty HCN liberated when the cake it´s flooded with 10 % HCL,...reading a lot how N2 or any inert gas atmosphere prevents cyanoborohydride descomposition and results on better yields......
After all,and thinking about my glassware possibilities and more,i decided to:
1.
Runned the reaction without N2 atmosphere.To minimize O2 and H2O on flask atmosphere,i used the smallest flask to make the reaction,so the air space on the top was minimal.After addition off all chemicals,read Ph(7) and closed very tigh the flask with aluminium foil and let it until reaction finished.
2.
Runned reaction without Ph adjusting.Have read Ph not change much with ammonium acetate vs more change with methylamine,thinking about how water makes yields go down,i decided to not put any 34 %Hcl to correct Ph because i´m lazzy
and seems there is not necesary with ammonium acetate.
So i describe how i runned that wonderfull experience
!
1.In a 1 litre flask,put in this order:
-
130 gr. ammonium acetate with
480 ml anhydrous methanol and stirred until all ammonium was on solution.Addition makes temperature falls
,so takes time to complete disolution.
-
28,4 gr. ketone.Solution becomes green.
-
8 gr. sodium cyanoborohydride.Weighted and trasnfered into the flask as soon as possible.
That amounts are Shulgin´s procedure X4.
2.Inmediatly covered the flask with aluminium foil very tigh and let stirring at medium tempo to create a minimum vortex on solution and let the atmosphere as quiet as possible.
3.
stirred at room tempo over 42 hours.Have read better yields becomes with 36 hours but need to extend to 42 hours because my work.Solution started clear yellow-green and the color intesity goes down to pale yellow almost water like colour until 42 hours.
3.Cheking Ph after addition of chemicals:was
Ph 7 when reaction finished was
Ph 7´5.Perfectly fine to cyanoborohydride activity.I was afraid about Ph changing,but no change during the reaction,and don´t wanted to let air and humidity go into reaction flask.
4.After 42 hours, put the flask on distillation setup,and distilled methanol under minimun vacumm,with air outlet of the vaccum pump conected to exterior.No gasses on the room and quickly methanol distilled .
5 .After methanol distillation,can see a very concentrated solution on the bottom of the flask,like 100 ml.
6. Let cold.No cake formed like some people tells.Thought was common on big batches with big amounts of ammonium acetate.
7.Make 600 ml 10 % Hcl and
poored into the flask using top of the 3- way adapter of distillation collum.Inmeadiatly,closed again the set-up quickly,but some nasty fumes scaped from the top.
Very very very nasty fumes .Happy only a little.Quickly connected vacumm on minimun to extract that gasses to exterior.That´s the more tricky part of reaction,but very easy anyway.
8.Let stir until no bubbling observed,like 30 minutes.Soution it´s milky green.
9.Extracted unreacted ketone with 100 ml DCM once.Very easy.DCM becomes green and solution becomes milky white without green tint.Saved the ketone/dcm to another batch.
10.Maked 250 ml Saturated Naoh solution and freezed.Transfered solution to a 1000 ml beaker and put into an ice bath with stirring.Basified that solution to Ph 13 very slowly.Funny bubbling again but no nasty fumes.Mda freebase was saw mostly on top and bottom on little drops form.
11.Extracted 2 times with 250 ml DCM:
Like fucking always,DCM on basic solutions made significant emulsions on my experiments.Will try next time with toluene to extract MDA freebase.When adding the dcm to the basic solution with stirring,becomes
red-wine!!.And
Dcm extractions were orange-red.12.Chilled DCM,and gassed with that guetto gasser from the forum made with a wash bottle.Really a improvement on gassing.Mixed like 100 gr calcium chloride and 50 ml 34% hcl,quickly covered,and almost instantlly hcl gas exist the tube in a very dry form.Gassed the solution until no more crystals precipitated.
That crystals on DCM are way more big and sparkly than the puffy ones of mdma on toluene.Really pretty preetty sparkly white crystals with little pink.13. Let deposite on bottom while chilling,filtered,acetone washed....
18 Gr MDA HCL on pretty sparkly smow white colour!
It´s a aprox. yield of 65 %.Much better than aprox. 35 % shulgins with 7 gr ketone.Very logical the bigger the batch,bigger the yield.Of course,it´s far from the 80-90 % Strike yields,but that it´s one of the most easiest reaction i have done.
Bad things:cyanoborohydride price!50 gr=185$.But thinking on only used 8 gr cyanoborohydide,that reactions sound now way better.
Didn´t tasted the product yet at this moment..
:DThat will be tomorrow Friday.Of course it will be a great night!
HOPE THAT MY EXPERIENCE CAN HELP SOMEONE TO DO THAT REACTION IF IT´S INTO HIS INTENTIONS.
BYE AND THANKS TO ALL!
(only have read it´s produced on the synthesis of Na cyanoborohydride from Na bororohydride)
MDA.Sodium Cyanoborohydride.zip