Hydrogen Sulfide → HCID 14536608, compound

Participants

Reaction Steps

A solution of 10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide, L series (6 g), and 3-methylbutylamine (18.9 cc) in absolute ethanol (90 cc) is saturated with hydrogen sulphide and brought for 16 hours to a temperature in the region of 105° C. After cooling, the reaction mixture is concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The oily brown residue is purified by chromatography on a column (height: 40 cm, diameter: 4 cm) of silica gel (0.02-0.063 mm), eluting with methylene chloride (1 liter) and then with a mixture (1.5 liters) of methylene chloride and methanol (95:5 by volume) and collecting 80-cc fractions. Fractions 23 to 36 are combined and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. N-(3-Methylbutyl)-10-[1-(1-pyrrolidinyl) -2-propyl]-2-phenothiazinecarboxamide, L series (6.76 g), is thereby obtained in the form of an orange-colored oil.

Provenance & Evidence