Methanesulfonic Acid → 3-Cyclopropylamino-3-methylazetidine dimethanesulphonate

Participants

Reaction Steps

14.5 g of 1-benzhydryl-3-cyclopropylamino-3-methyl-azetidine in 150 cm3 of methanol are hydrogenated at atmospheric pressure and at a temperature in the region of 20° C. for 1 hour in the presence of 5.6 g of 20% palladium hydroxide on carbon. The reaction mixture is treated with 10 g of methanesulphonic acid. After removal of the catalyst by filtration and concentration to dryness under reduced pressure (20 kPa) at approximately 40° C., the residue is washed with 3 times 150 cm3 of ethyl ether. The final residue is taken up with 100 cm3 of 2-propanol, drained and washed with twice 50 cm3 of acetone. 9.1 g of 3-cyclopropylamino-3-methylazetidine dimethanesulphonate are obtained in the form of a colorless solid, melting point 136° C.

Provenance & Evidence