1-Methylpiperazine → HCID 3045791, Verbindung
Reaktionsgleichung
[F:1][C:2]([F:21])([F:20])[C:3]1[C:18]([Cl:19])=[CH:17][C:6]2[CH:7](Cl)[CH2:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[S:11][C:5]=2[CH:4]=1.[CH3:22][N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1>C(Cl)(Cl)Cl>[F:1][C:2]([F:21])([F:20])[C:3]1[C:18]([Cl:19])=[CH:17][C:6]2[CH:7]([N:26]3[CH2:27][CH2:28][N:23]([CH3:22])[CH2:24][CH2:25]3)[CH2:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[S:11][C:5]=2[CH:4]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A mixture of 7-trifluoromethyl-8,10-dichloro-10,11-dihydrodibenzo(b,f)thiepine (2.89 g), 1-methylpiperazine (1.8 ml) and chloroform (2.5 ml) was refluxed for 7 hours. The chloroform was evaporated under diminished pressure, the residue dissolved in benzene (30 ml), washed with water, and the benzene layer separated and shaken with an excess of 3 N-HCl. The precipitated hydrochloride was filtered, added to the aqueous layer of the filtrate and the base liberated by addition of ammonium hydroxide. It was extracted with benzene and the conventional work-up procedure yielded 1.93 g (56%) of the crude 7-trifluoromethyl-8-chloro-10-(4-methylpiperazino)-10,11-dihydrodibenzo(b,f)thiepine. Neutralization with maleic acid in ethanol followed by addition of ether yielded the crystalline maleate which was crystallized from ethanol; m.p. 197°-200° C.