2-Cyclopropylethan-1-ol → HCID 54557695, compound

Participants

Reaction Steps

A mixture of 3.45 g (10 mmol) of ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate, 0.17 g (0.72 mmol) of tetraethyl orthotitanate and 7.5 g of 2-cyclopropyl-ethanol is stirred at 130° for 14.5 hours, about 2 ml of solvent being distilled off after 0.5 hour. The mixture is subsequently evaporated to dryness in vacuo, the residue is taken up in chloroform and chromatographed on silica gel while eluting with ethyl acetate. After crystallization of the resulting oil from ethyl acetate/n-hexane, there is obtained 2-cyclopropylethyl (S)-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 163°-164°.

Provenance & Evidence