1-Methylpiperazine → HCID 12271965, compound

Participants

Reaction Steps

A mixture of 7,8-difluoro-10-chloro-10,11-dihydrodibenzo(b,f)thiepine (5.08 g), 1-methylpiperazine (4 ml) and chloroform (5 ml) was refluxed for 7 hours. Chloroform was evaporated and the residue shaken with water and benzene. The organic layer was washed with water and shaken with dilute (1:2) hydrochlorid acid (50 ml). The formed suspension was filtered and the thus-obtained solid hydrochloride added to the aqueous layer of the filtrate. Addition of 15% sodium hydroxide solution liberated the desired base which was extracted with benzene, m.p. 106°-108° C. (acetone). Neutralization of this base with methanesulfonic or maleic acid in ethanol, followed by the addition of ether, yields the corresponding salts, i.e., the methanesulfonate (m.p. 244°-247° C.) or maleate (hemihydrate, m.p. 161°-163° C.), which were purified by crystallization from a mixture of ethanol and ether.

Provenance & Evidence