Hydrochloric Acid → HCID 13631914, compound

Participants

Reaction Conditions

Reaction Steps

0.6 g (0.0016 mole) of 7-chloro-5-phenyl-1'-methyl-spiro[1H-1,4-benzodiazepine-3,4'-piperidin]-2(3H)-one are dissolved in 15 ml of absolute dimethylformamide and reacted with 0.1 g of sodium hydride (55-60% strength dispersion) at 70° C. After 30 minutes, the mixture is cooled to 25° C., 0.22 g (0.0016 mole) of methyl iodide in 10 ml of absolute dimethylformamide is added and the mixture is stirred for 2 hours. After the solvent has been distilled off, the residue is taken up in water and the mixture is extracted with methylene chloride. For purification, the product is chromatographed on aluminum oxide 90 (Merck), activity level II-III, with a cyclohexane/methylene chloride/methanol mixture (6:3:1), and the base thus obtained is converted into the hydrochloride by treatment with diethyl ether/HCl.

Provenance & Evidence