Methanol → HCID 24969354, compound

Participants

Reaction Steps

In a mixture solvent (methanol:water=6:1) (0.7 ml) was dissolved (3R)-1-isobutyl-7-chloro-5-(2-chlorophenyl)-2,3-dihydro-2-oxo-1H-1,4-benzodiazepine-3-acetic acid (30 mg) obtained in Example 13. To the solution was added sodium borohydride (10 mg). The reaction mixture was stirred for two hours at room temperature, to which were added dichloromethane (50 ml) and water (50 ml). The aqueous layer was made acid, then the organic layer was washed with a saturated aqueous saline solution, followed by drying over anhydrous sodium sulfate. The solvent was removed, and the residue was recrystallized from dichloromethane/petroleum ether to give 17 mg of colorless crystals, m.p. 184°-188° C.

Provenance & Evidence