Water → 1-methyl-cyclopentyl 8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate

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Reaction Steps

1.2 g (12 mmol) of 1-methyl-cyclopentanol in 25 ml of dry dimethylformamide is treated with 0.5 g (10.3 mmol) of sodium hydride (55% oil dispersion) and to the resulting solution there are added portionwise at -20° 3.79 g (10.3 mmol) of (S)-1-[(8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-1-yl)carbonyl]imidazole. The mixture is stirred at room temperature for 1 hour, poured into about 250 ml of water, the precipitated material is filtered off under suction, washed with water and dried. There is obtained 1-methyl-cyclopentyl 8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 190°-191°.

Provenance & Evidence