Methyl iodide → HCID 13631918, compound

Participants

Reaction Conditions

Reaction Steps

3.0 g (0.0069 mole) of 7-chloro-5-phenyl-1'-benzyl-spiro[1H-1,4-benzodiazepine-3,4'-piperidin]-2(3H)-one are dissolved in 25 ml of absolute dimethylformamide, and 0.3 g (0.007 mole) of sodium hydride (55-60% strength dispersion) is added at 20° C. After the mixture has been stirred for 20 minutes, it is cooled to 0° C., a solution of 1.0 g (0.0065 mole) of methyl iodide in 5 ml of absolute dimethylformamide is added dropwise and the mixture is stirred at 25° C. for 3 hours. The solvent is distilled off and the residue is purified by column chromatography over silica gel 60 (Merck). After the column has been eluted with methylene chloride/methanol (9:1), the oily base is obtained, which slowly crystallizes completely. Colorless crystals of melting point 169°-170° C.

Provenance & Evidence