1-Methylpiperazine → HCID 3045477, compound

Participants

Reaction Steps

1-Methylpiperazine (18.2 ml) was added to a solution of 7-chloro-8-fluorodibenzo(b,f)thiepine-10(11H)-one (see Example 24) (10.16 g) in benzene (90 ml). To this mixture a solution of titanium tetrachloride (3.7 g) in benzene (30 ml) was added dropwise during 5 minutes. The mixture was refluxed for 24 hours, cooled and decomposed by addition of ice-cold water (150 ml). After 30 minutes' standing, the precipitated solid was filtered and washed with benzene. The aqueous layer of the filtrate was extracted with the same solvent, the benzene layers combined, washed with water, dried and taken down, leaving 12.1 g (91%) of the oily base which slowly crystallizes from ethanol. When pure, it melts at 158°-160° C. Neutralization with maleic acid in ethanol yielded the crystalline maleate, m.p. 228°-230° C. (aqueous ethanol).

Provenance & Evidence