3,4mdp2np reduction

[amieri]

Hope all is well with everyone . Id like to gather some peoples opinions.
I don't ever come across much on MDA purification on this forum or any of the others. Although similar to amphetamine in many ways I have read unlike amph MDA can't be steamed distilled , if this is true my first question is. What is the science behind why it can't be ?
Now let's say mdp2np was reduced via al/hg , basing to a ph of 11 and collection/drying "mgs04" what do y'all like to do? Directly salting with acetone/h2so4 has lead to some really waxy questionable product. Recrystallation in IPA twice left a fluffy white powder.
My next thought was vacuum distillating the solvent off then resolving in acetone and salting same as before which left a still somewhat waxy product that recrystallized same as before.
Id like to try a/b washing and fractional distillating of the fb.my question is with 10 gram reductions of propene do I need a micro distillation set? Also how does the fb come over? Is it a bumping/jumping type thing or will it actually turn to a vaper ? Any pointers,tips or suggestions are greatly appreciated.
You all please stay amazing and be safe.thanks in advance

 

[HIGGS BOSSON]

We will soon have a video on the synthesis of MDA from helional, and there we will show the methods of purification.
As far as I remember, the processes with MDP2np went the same way as with p2np

 

[amieri]

I check every morning for it ,can't wait higgs you all are such inspirations thanks for being u

 

[Rabidreject]

I am reducing some md-p2np right now using the NaBH4 / CuCl2 method.
If it works a fraction as well as my 3,4,5-TMONS worked, I’ll be happy and will let you know.
I’m not hugely surprised you needed to re-x it though, particularly if you didn’t re-x the md-p2np before reducing. (Only because I know where you got your md-p2np from!)

Im looking up methods of converting to the phenylacetone now tbh.

Would a simple alkaline hydrolysis work do you think?

I'm not even really sure why I’m messing around with this - I really don’t even like to take any of the MD compounds! Ha
It just seems like something I should synthesise…and I’m not sure why!

 

[w2x3f5]

reaction with tin chloride and hydrochloric acid in ethyl acetate, on simple p2np worked well.

 

[Rabidreject]

Conc HCl? Interesting I’ll look into it

 

[Rabidreject]

Edit: commented in the wrong place…

 

[w2x3f5]

I copied with erowid, hydrochloric acid can be used diluted, it works great on the usual P2NP:

18.1g (100mmol) 1-(2-fluorophenyl)-2-nitropropene was added dry in portions to 49.5g (220mmol) SnCl2·2H2O suspended in 75ml EtOAc while the reaction temperature was kept between 20-40°C by a cold water bath. When all nitropropene was added and the color had changed to white (5 min) the EtOAc solution was transferred to a RB flask containing 250ml water and 50 ml hydrochloric acid. The EtOAc was removed by distillation under diminished pressure and the aqueous suspension of oxime and tin salts was allowed to stir at 80°C for 1 hour. The water phase was now steam distilled to remove the ketone. When no more oily drops came over the distillate was extracted with DCM. The DCM extracts was dried over MgSO4 and the DCM removed by distillation leaving a quite pure ketone as a colorless oil.
Yield: 13,5g (89%) 1-(2-fluorophenyl)-2-propanone
Purity: 98% (HPLC)
Properties: bp 47°C/0.05 mmHg, d 1.077g/ml (according to the Aldrich Catalog).

 

[Rabidreject]

I am also interested if u can steam distill the freebase of MDA.
Guessing not as you can’t other substituted ones like mescaline but why?