One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

MadHatter

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Also, something strange:
I saved the black slurry part of the reaction mixture, and combined it with the aqueous layer from the freebase separation. Poured in a bunch of acetone and left it standing overnight in a temperature just above freezing.
When I came to fetch it this morning there was the expected clear layer on top, but the bottom layer was SOLIDIFIED with clear, rock hard crystals. So hard the have to be chiseled loose. I tried solving some of them in tolune, acetone and water, but they're insoluble. The crystals themselves are clear as ice, but they.ve formed around the black nanoslurry of the CuSO4.
See attached picture taken into the beaker.
What on earth could this be?
 

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MadHatter

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After giving it some thought and a bit of experimentation, I'm pretty sure these are borate crystals. They dissolve just fine in warm acidified water.
 

WinterDust

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@MadHatter, jesus christ this has annoyed me for a long time, but I can finally put it into rest.

You are correct, the "sludge" is borate crystals from the NaoH, I just did another reaction and the outcome was exactly the same.

Best regards
 

JIW_LWB

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Would this work also with cas 1451-82-7 2-bromo-4-methylpropiophenone ?

(I’m a rookie but supplier is stating it’s the same, in my logic it is isn’t )
 

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G.Patton

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Hello, this method works for reagent list, which is described in the post. 2-Bromo-4-methylpropiophenone is 4-MMC precursor.
 

JIW_LWB

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Ok good that you mention! Should’ve taken more time reading patiently.. good to know it’s for 4mmc only thing is another option I’m interested in … wished payed more attention in school during chemistry 😭
 

aa1178251182

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Can amphetamine be made into crystals like this?
 

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WinterDust

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Yes and No.

Amphetamine is a powder state substance, what you have in the picture is Chrystal Methamphetamine.

There is a route here on the forum on how to synthesize Methamphetamine from Amphetamines, check it out.

Best regards
 

henwest

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Where can i find nabh4 in Holland
 

Saul

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@henwest laboratoriumdiscounter google it
 

aa1178251182

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Only 60% sulfuric acid can be purchased, can it be used for crystallization?
 

tucoXxX

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I want to buy cooling and heating equipment. should it work together with the reactor? or should I buy a separate one? 1kg will be p2np synthesis, I am trying to make a-oil.
 

blackburn

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You need both cooling and heating for this, What kind depends on equipment.
 

tucoXxX

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30L jacket glass reactor .
20L rotary evaporator.
Heat _ chiller -30C to 200C.
reactor and cooling-heating equipment work together continuously during work? Does this refrigerator-heater correspond to what I wrote?

Gdx -30/30 heater and chiller
 

tucoXxX

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p2np -->a-oil end product . I would like to know exactly what equipment is needed. The seller has questions, but unfortunately I don't understand what he is asking. for making a larger batch. first a small lot, then a big one. 30L double jacketed reactor. Rotary evaporator 20L. GDX-30/30 30L tank volume Heather chiller (this works together with a reactor), I think a smaller one is sufficient instead. DLSB-20/30 Recirculating chiller do I also need this for synthesis??? isn't the fridge-heater enough? SHB-B95 vacuum pump is required as far as I know. I would like to buy the tools, but before that, advice on how to make them perfect
 

gcblin

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Can someone explaine this white layer at the bottom i finished adding p2np to nabh4
 

WinterDust

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Hi,

What do you mean by "Finnished adding P2nP to NaBH4"?

You ad P2nP to the reaction mixed with IPA + H2O + NaBH4.

The NaBH4 settles at the bottom of the reaction if you stop stirring it will "rock up".

Best regards
 

gcblin

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Yeah everything was addet properly i was worried about the white layer, soon i will be finishing up will post result photos
 

MadHatter

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Yup, like the man said, it's borate crystals. Also, if you leave the rm cooling overnight for some reason, ice-like boric crystals will aggregate at the bottom. Like a small glacier. I got this on a massive scale at my first run and really wondered what i was looking at. Tested, and drew the conclusion it had to be boric crystals.
 
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