Diisopropyl Ether → HCID 14536543, compound

Participants

Reaction Conditions

Reaction Steps

Mercuric aoetate (I.8I g) dissolved in glacial acetic acid (35 cc) is added in the course of 20 minutes to a solution of 10-[(2RS)-1-(perhydro-1-azepinyl)-2-propyl]-N-propyl-2-phenothiazinecarbothioamide (2.5 g) in acetic acid (25 cc), and the mixture is stirred for 45 minutes at a temperature in the region of 20° C. The black suspension obtained is filtered on sintered glass plugged with celite, and the yellow filtrate is concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residue is taken up with ethyl acetate (250 cc) and distilled water (50 cc). The organic phase is washed successively with normal sodium hydroxide (2×100 cc) and distilled water (3×100 cc) and with saturated aqueous sodium chloride solution (100 cc) and dried over magnesium sulphate. After filtration, the yellow filtrate is concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C. and a crude yellow oil (2.1 g) is thereby obtained This residue is taken up with boiling isopropyl ether (80 cc). The small amount of insoluble matter is removed by filtration and crystallization is primed in the filtrate by cooling maintained with stirring. The crystals are filtered off on sintered glass to give 10-[(2RS)-1-(perhydro-1-azepinyl)-2-propyl]-N-propyl-2-phenothiazinecarboxamide (1.29 g) in the form of an offwhite solid, m.p. 113° C.

Provenance & Evidence