foxy2
(Hive Addict)
09-05-01 20:47
No 210412
      MDE from Safrole Azide
(Rated as: excellent)
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This procedure looks like it would work for MDE.
Later
Foxy

Use Ritter's procedure with bromosafrole to make the azide.
../rhodium/chemistry /mda.azide.html

To convert the azide to MDE.
Instead of extracting the azide with toluene use xylene. Use a dryed xylene extract in the following procedure.

Example using cyclopentyl azide.

In a dry 50ml flask equiped with septum inlet, reflux condenser, and magnetic stirrer was flushed with nitrogen.  The flask was charged with 10mL xylene and 0.98g, 1.42ml(10 mmol) of triethylborane.  The solution was then heated to reflux and attached to a gas buret.  Then 1.11g (10 mmol) cyclopentyl azide was added.  After completion of nitrogen evolution, the flask was cooled, 30 ml diethyl ether was added and the amine extracted with 6 M HCl, two 20 ml portions.  The aqueous phase was then washed with ether to remove residual borinic acid.
Yeild 77%

The reaction of represetative organic azides with triethylborane.  A new route to secondary amines.
J. Am. Chem. Soc.
93:17, 4329-4330 (1971)

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    Rhodium
(Chief Bee)
09-05-01 20:52
No 210413
      Re: MDE from Safrole Azide  Bookmark   

Triethylborane (NASTY!) forms ethylamines with azides, is that what you say?
 
 
 
 
    foxy2
(Hive Addict)
09-05-01 22:18
No 210443
      Re: MDE from Safrole Azide  Bookmark   

Thats what the article is saying.  The steric hinderance of safrole azide may lower the yeild.

I never said triethyl borane was nice to work with. tongue


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    Ritter
(Master Whacker)
09-13-01 06:35
No 212907
      Re: MDE from Safrole Azide  Bookmark   

MDE is a bastardized derivative of MDA and MDMA.  It tends to make about 1 in 4 people sick, has a short duration of action, lacks any and all empathetic qualities its mentioned congeners possess and flat out is a waste of good ethylamine.  Not to mention one has to consume close to 170mg to experience any effects at all. This stuff is a total waste of time.