Ethanol, reaction products with ammonia, distn. residues → HCID 11127710, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of (2-methoxy-6,7,8,9-tetrahydro-5H-benzocyclohepten-9-ylidene)acetonitrile (2.00 g, 9.38 mmol) in ethanol (10 ml) were added a saturated solution of ammonia/ethanol (5 ml) and Raney nickel (W-2, 2 g). The mixture was stirred for 4 hours at 50° C. under hydrogen atmosphere (4 kgf/cm2). The Raney nickel was filtered off, then the solvent was distilled off under reduced pressure. The residue was purified by means of a silica gel column chromatography (chloroform:methanol=9:1 to chloroform:methanol:triethylamine=90:8:2) to give the above-titled compound (1.50 g, yield 74%, oil).

Provenance & Evidence