Cyclohexanol → HCID 22828757, compound

Participants

Reaction Steps

A mixture of 4.0 g (10 mmol) of tert.butyl (S)-8-chloro-7-fluoro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate, 0.8 g (3 mmol) of tetraethyl orthotitanate and 15 ml of cyclohexanol is stirred at 120° overnight, evaporated to dryness, the residue is taken up in methylene chloride, the solution obtained is washed successively with 40 ml of 5N hydrochloric acid, water and saturated sodium bicarbonate solution, dried over magnesium sulphate and evaporated. There is obtained cyclohexyl (S)-8-chloro-7-fluoro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 163°-166°.

Provenance & Evidence