Question Stupid question about MDA from helional.

HIT MONKEY

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Hello friends I'm a newbie and don't know much about chemistry.
Stupid question=I have synthesized MDA from helional through a reaction.
The aldoxime of this aldehyde undergoes Beckman rearrangement with nickel acetate to yield an amide. which are then converted to amines by the Hoffman reaction.
(Note)=The last step is How do I sharpen my crystal?
 

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The solution was cooled and extracted with xylene. The solution was filtered and the filter was washed with xylene and the xylene fraction added together. Then, approximately 100 mL of concentrated HCL was added to the shaken xylene and separated. An aqueous solution is also extracted. Xylene and xylene are separated. The amine is then released from the aqueous phase with NaOH.
What is the final step after adding NaOH? So what method should I use to crystallize mda crystals and what is the PH?
 

The-Hive

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theres a video on here that shows how to do that but id do it the same way the first time round. PH 7

 

HIT MONKEY

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You mean this one?=
The amines are then released from the aqueous phase with a NaOH solution (45 g of NaOH in 135 mL of water). The oil is separated with ether (or toluene, methylene chloride, etc.). It is then converted to HCl salts along the HCl gas stream. The crystals formed from the ether are filtered out.

Am I understanding this correctly or is it wrong?
=Thank you
 

skarlett

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who in europe that can do this and would like to meet up? - i got everything but dont know how to do it. - anyone?
 

The-Hive

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No face no case 👌🏻
 
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HIT MONKEY

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I failed at the last step.
And I don't know how to crystallize MDA from the aqueous phase.
 

HIT MONKEY

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I've checked out the tips and how-to from The-Hive.
And I found different ways. Plenty to crystallize it. But I don't know what to do next.
 

HIT MONKEY

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I'm sorry, but I really don't know what to do.
And in my country there is not much knowledge about chemistry.
I'm sorry for how stupid my question was. But I need help and want to know what I need to do and what to do next.

Thank you for the answer.
 
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