Water → HCID 13280937, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 4.0 g (9.6 mmol) of 8-chloro-6-(2-chlorophenyl)-1-methyl-2H,4H-pyrrolo[3,4-d][2]benzazepine-2-acetic acid methyl ester in 40 ml of tetrahydrofuran was added dropwise to a solution of 0.8 g (21.0 mmol) of lithuium aluminum hydride in 50 ml of tetrahydrofuran which was cooled to -78° C. When the addition was complete, the reaction mixture was allowed to warm to 0° C. and stirred for 30 minutes. The mixture was treated with 1 ml of water, 1 ml of a 3 N solution of aqueous sodium hydroxide and 3 ml of water. The resulting precipitate was removed by filtration, and the filtrate was concentrated at reduced pressure. The residue crystallized from ether to yield 8-chloro-6-(2-chlorophenyl)-1-methyl-2H,4H-pyrrolo[3,4-d][2]benzazepine-2-ethanol as pale yellow prisms, mp 149°-152° C. Recrystallization from a mixture of ether and methylene chloride gave white prisms, mp 151°-153° C.

Provenance & Evidence