Ammonium Chloride → HCID 20433756, compound

Participants

Reaction Steps

2.7 gm (6 mmols) of 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-[N-methyl-N-(2-{3,4-dimethoxy-phenyl}ethyl)-amino]-propane were dissolved in 100 ml of absolute ether and 100 ml of absolute tetrahydrofuran; the solution was mixed with 0.25 gm of lithium aluminum hydride, and the mixture was refluxed for 3.5 hours. After cooling, a 10% ammonium chloride solution was added, while cooling was continued; then the mixture was suction-filtered, and the filtrate was concentrated by evaporation. The residue was purified on a silica gel column with methylene chloride. The fractions were concentrated by evaporation, the residue was dissolved in acetone, and the dihydrochloride was precipitated with methanolic hydrochloric acid.

Provenance & Evidence