This procedure looks like it would work for MDE.
Later
Foxy
Use Ritter's procedure with bromosafrole to make the azide.
https://www.thevespiary.org/rhodium/Rhodium/chemistry/mda.azide.html (https://www.thevespiary.org/rhodium/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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