C-(3,4-DIMETHOXY-BICYCLO[4.2.0]OCTA-1(6),2,4-TRIEN-7-YL)-METHYLAMINE synthesis

Yield: 100%

Reaction Conditions:

with ammonia;hydrogen;nickel in methanol at 60; under 22502.3 Torr;Industry scale;

Steps:

1.A
Introduce 4,5-dimethoxy-1-cyano-benzocyclobutane (6 kg), methanol (30 litres), Raney nickel (0.6 litres) and ammonia (7.32 kg) into a hydrogenator. After having purged with nitrogen and then with hydrogen, hydrogenate at 60° C. and at 30 bar until the theoretical amount of hydrogen has been absorbed. After returning to 20° C., filter off the catalyst, rinsing it with methanol, and then evaporate off the solvent. The title compound is obtained in the form of an oil, in a quantitative yield.

References:

Lerestif, Jean-Michel;Blanco, Isaac Gonzalez;Lecouve, Jean-Pierre;Brigot, Daniel US2005/261376, 2005, A1 Location in patent:Page/Page column 3