Cloxazolam → HCID 21442401, compound

Participants

Reaction Steps

A solution of 2.8 g. of 10-chloro-11b-(2-chlorophenyl)-2,3, 5,11b-tetrahydrooxazolo[3,2-d] [1,4]benzodiazepin-6(7H)-one in 50 ml. of dimethylformamide was cooled to -10° and treated with 0.65 g. of sodium methoxide. After stirring for 5 minutes, the mixture was cooled to -40° and 1 ml. of chlorodimethyl ether was added. The cooling bath was removed and when the temperature had reached 0° the reaction mixture was poured into 300 ml. of ice-water. The precipitated material was collected by suction and dissolved in methylene chloride. The solution was dried over sodium sulfate, filtered and evaporated. The residue was crystallized from a mixture of ether and hexane to give, after recrystallization from ethanol, 10-chloro-11b-(2-chlorophenyl)-7-methoxymethyl-2,3,5,11b-tetrahydrooxazolo[3,2-d][1,4] benzodiazepin-6(7H)-one as white prisms, m.p. 14 4°-147°.

Provenance & Evidence