Acetic Acid → HCID 12440687, compound

Participants

Reaction Steps

A solution of 13.3 parts of 2-methylthio-4-phenyl-3H-1,5-benzodiazepine, 26 parts by volume of 1-methylpiperazine and 1.5 part of glacial acetic acid in 150 parts by volume of chloroform is stirred at reflux temperature overnight. The solvent is then removed under reduced pressure and the residue partititoned between water and benzene. The benzene portion is washed with water and then extracted with 10% acetic acid. The acidic extract is washed with benzene and then made alkaline with concentrated ammonia. The alkaline mixture is extracted with benzene, the benzene extract washed with water and then dried over anhydrous magnesium sulfate. After the solvent is removed a crude yellow solid is obtained. The crude solid is recrystallized from a mixture of chloroform and n-hexane to yield 4-(4-methyl-1-piperazinyl)-2-phenyl-3H-1,5-benzodiazepine, melting at about 155°-157° C. This compound has the following formula ##STR16##

Provenance & Evidence