Cyclohexanol → HCID 20434837, compound

Participants

Reaction Steps

A mixture of 8.72 g (27 mmol) of ethyl-7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate, 2 g (9 mmol) of tetraethyl orthotitanate and 27 g (270 mmol) of cyclohexanol is stirred at 125° overnight, evaporated to dryness, the residue is taken up in chloroform, the chloroform solution is washed successively with 40 ml of 5N hydrochloric acid and saturated sodium bicarbonate solution, dried over magnesium sulphate and evaporated. By recrystallization from ethanol and ether there is obtained cyclohexyl 7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 208°-209°.

Provenance & Evidence