Flumazenil → HCID 20434833, compound

Participants

Reaction Steps

A mixture of 20.0 g (65.9 mmol) of ethyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate, 1.0 g (15.4 mmol) of potassium cyanide and 100 ml of propargyl alcohol is stirred at 125° for 20 hours and at 135° for 1 hour, evaporated to dryness in vacuo and the residue is taken up in chloroform. The chloroform solution is washed twice with water, dried over magnesium sulphate and evaporated. The residue is chromatographed on silica gel while eluting with ethyl acetate. By recrystallization of the resulting material from chloroform/toluene there is obtained 2-propynyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 220°-222°.

Provenance & Evidence