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Author Topic: small batches on reductive amination with NA cyanoboro. and ammonium acetate  (Read 357 times)

lugh

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Re: small batches on reductive amination with NA cyanoboro. and ammonium acetate
« Reply #20 on: September 29, 2010, 01:35:42 AM »
There's no need to gas distilled mda free base with hcl, it can be crystallized if one has reagent grade aqueous hydrochloric acid and the resulting crystals washed with acetone if one doesn't have diethyl ether  8)
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jon

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Re: small batches on reductive amination with NA cyanoboro. and ammonium acetate
« Reply #21 on: September 29, 2010, 02:57:02 AM »
acetone always cleans it up nicely i've gotten white crystals just washing titrated mixture of mda base with stoichiometric glacial acetic acid.

sassa

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Re: small batches on reductive amination with NA cyanoboro. and ammonium acetate
« Reply #22 on: September 29, 2010, 01:59:06 PM »
Thank´s again jon for your help JON,lugh,... ;) ;)
   Proved yesterday recrystalization-evaporation of mda hcl from anhidrous methanol,making a supersaturated solution and let evaporate rest along night... and this morning what i have seen ::)....pretty big transparent crystals ,biggers than ones from mdma and almost dry on 1 night!.Definitly mda hcl wants methanol(or other alcohol) to evaporate from tand without fan to make big crystals.Must avoid try to obtain it by water evaporation.Sure all days i learn something  about that tricky things on crystallization.The crystals from methanol are awsome!.
    Fine that information about tricloroetane,but i´m on the way now of consume all my solvents and chemicals,so like i hate dcm to extract and proved don´t work well on my reactions,i´m going to extract the unreacted ketone from this final batch with dcm(never has problems on acid solutions), and then, the mda freebase from basic solution with toluene(worked ever easy on basic solutions).Of course i will run a last AL/Hg with that ketone and then...BYE CHEMISTRY!
« Last Edit: September 29, 2010, 02:10:09 PM by sassa »

sassa

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Re: small batches on reductive amination with NA cyanoboro. and ammonium acetate
« Reply #23 on: October 01, 2010, 03:59:48 PM »
Finally,72 gr. MDA HCl from 115 gr ketone(62 % yield)  using helium atmposphere refilled 2 times and with 36 hours  reaction time so...:
    -seems using inert atmosphere doesn´t increase yileds too muuch since sodium cyanoborohydride it´s on molar excess on most recipes.
     -seems working with big batches vs small batches it´s a good alternative about time but not too much about yields.Possibly more lazzy actitude about extractions and more this time,but the yield it´s aprox. the same..
      -the recovered unreacted ketone doesn´n look very good,because color turned darker and smell changed.Possibly a good amount degrades during process and it´s not usuefull to another batch.But will try to reduce it with Al/hg and nitromethane.
       -have read using silica gel beads during reaction  increase yields on 25%,but not proved.

   
   

sassa

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Re: small batches on reductive amination with NA cyanoboro. and ammonium acetate
« Reply #24 on: October 08, 2010, 01:27:50 AM »
i promisse this is my last post on this thread. ;D
   Only talk about proved that pure mda,without combination with mdma and have to say it´s the funniest drug i have taken to go party(sure incredibles nights with friends at home,but posibly to do that maybe better with mdma.

I noticed substancial diferences from mdma experiences,most of it making mda more funny and plenty to make party than mdma:
   1º:I have noticed after the first doses taking an incredible need to do things and to speak with my friends. But especially to do things. Under the influence of the mda any situation turns into an extraordinary experience.
     The first night in mda, a friend of mine and I were in the door of a dance bar in full  high peak ;D, and we saw that to the side was a left house. I was bringing in my turnkey a small lantern, and we end inspected the terrific house completely in the dark, with only the help of the small lantern, and for more amazement, all the rooms of the house were in the style of the scenes of the movie "saw":Really darkly, but my friend and I was feeling that not any bad thing could suffer to us, and we devote ourselves to enjoy of the experience without any fear.Probably sound infantile (I have 34) counted this way, but under the influence of the mda, it was one of the experiences mas fascinating that I have had!.

    I feeld the mdma experiencie like most comtemplative and little mystical.Anyway,all that fellings were there,but with the need of esperimente all aspects and forms of the nature and peolple all around.

 2:the high it´s more progresive and long,so you don´t feel are getting high..it´s like that feelings are inside you,and not so articial like mdma feelings can be(loving a person for example you really know you
hate and it´s a bad person :D).There is no more need to redose since you didn´t feel waves,you simply go up and down along the night in a very natural way.

3.The nights are more longer and more intense.Last night i did it,came to house to sleep at 17:00 in the afternoom! :owithout any feel of sleep or hungry.

4.The day after and more,the feeling it´s like you are exhausted,very very tired,but without any mental comedown like semidepression.You are tired,but with the feeling the night and experiences were great.

5.To my amazement,i didn´t notice any visuals.Only like said some colors more bright or full,but no figure withou closed eyes and any tipical from mda experiences.A suposse my lot of experiences with mdma would be responsable of that.

   General,a great drug that is growing on me.I´planning  to do it fewest times possible,because i don´t want to lost any magic like happened with mdma.of course,i´m planning do that to with mdma,because last times was a little disaponted about the experiences.Possibly,it´s hard to make all nights unforgeateble. :'(.
    Bye and best hopes to all.!
   Were great all experiences i had while reading and posting on this forum.Very friendly peolple here. ;) ;) ;)
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