Ammonia → HCID 67918524, compound

Participants

Reaction Steps

0.70 g (0.0014 mol) of 3-[(N-(2-(3,4-dimethoxy-phenyl)ethyl)-piperidin-3-yl)-methyl]-7, 8-dimethoxy-1,3,4,5-tetrahydro2H-3-benzazepin-1,2-dione are dissolved in a mixture of methanol and water (95:5), 0.060 g (0.0016 mol) of sodium borohydride are added and the mixture is stirred for 20 minutes at ambient temperature. Then it is acidified with 2 molar hydrochloric acid, neutralized with ammonia and extracted with methylene chloride. The organic phase is dried over magnesium sulphate, concentrated by evaporation in vacuo and the residue obtained is purified over 100 g of aluminium oxide (neutral, activity II-III) with methylene chloride and then with increasing amounts of ethanol (up to 15%). The hydrochloride is precipitated from a solution in acetone using methanolic hydrochloric acid.

Provenance & Evidence