1-Methylpiperazine → HCID 3045486, compound

Participants

Reaction Steps

A mixture of 7-fluoro-8,10-dichloro-10,11-dihydrodibenzo(b,f)thiepine (7.48 g), 1-methylpiperazine (5.2 ml) and chloroform (7 ml) was refluxed for 7 hours. The chloroform was evaporated and the residue taken up in water (20 ml) and benzene (80 ml). The benzene solution was washed with water and shaken with 3 N-HCl (100 ml). The separated hydrochloride was filtered and added to the aqueous layer of the filtrate. The resulting suspension was made alkaline with ammonium hydroxide and the liberated base taken up in benzene. The desired product, m.p. 105°-107° C. (acetone), was obtained in 74% yield (6.66 g). Its neutralization with maleic acid in ethanol, followed by addition of ether, yielded the crystalline maleate, m.p. 168°-169° C. (ethanol).

Provenance & Evidence