Hydrochloric Acid → HCID 15925248, compound

Participants

Reaction Steps

Propylamine (0.75 cc) is added to a solution of 7-chloro-10-[(2RS)-1-diethylamino-2-propyl]-2-phenothiazinecarbothioamide (0.6 g) in absolute ethanol (5 cc). The mixture is brought to 200° C. for 4 hours and then diluted with ethyl acetate (50 cc), washed with distilled water (2×100 cc), dried over magnesium sulphate and then concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residual solid is purified by chromatography on a column (height: 8.5 cm; diameter: 2 cm) of silica gel (0.6-0.02 mm), eluting with a 20:80 (by volume) mixture (1.5 liters) of ethyl acetate and cyclohexane, collecting 30-cc fractions. Fractions 25 to 36 are combined and concentrated under reduced pressure (30 mm Hg; 4 kPa) to give a brown oil, which is dissolved in ethyl ether (10 cc). 2.2N ethereal hydrochloric acid (2 cc) is added to this solution. The suspension obtained is filtered to give 7-chloro-10-[(2RS)-1-diethylamino-2-propyl]-N-propyl-2-phenothiazinecarbothioamide (0.06 g), m.p. 130° C.

Provenance & Evidence