1-Methylpiperazine → HCID 12521666, compound

Participants

Reaction Steps

A solution of 0.7 g. of 6-chloro-10-(methylthio)-4H-thieno[3,4-b][1,5]benzodiazepine in 3.5 ml. of N-methylpiperazine is treated with 1-2 drops of glacial acetic acid and heated under reflux for 4 days. The solution is concentrated to dryness and the residue is warmed with dilute acetic acid. The acidic solution is filtered, cooled, and made alkaline with concentrated ammonium hydroxide. The precipitate is collected, washed with water and recrystallized from acetone-petroleum ether (30°-60° C.) to give yellow crystals, m.p. 148°-149° C. (dec.).

Provenance & Evidence