反应详情

温度

20 °C

A solution of N-propyl-10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide, L series (5.5 g), in acetone (15 cc) is introduced, dropwise and with stirring during 30 minutes, into a solution of methyl bromide (9.5 g) in acetone (90 cc), and stirring is maintained for 16 hours at a temperature in the region of 20° C. The suspension obtained is filtered and the solid is washed with acetone (3×1 cc), drained and dried at 40° C. under reduced pressure (5 mm Hg; 0.7 kPa). This amorphous white solid (4.8 g) is dissolved in acetonitrile (12 cc) under reflux. The crystals formed after cooling are drained, washed with ice-cold acetonitrile (3×3 cc) and dried at 40° C. under reduced pressure (5 mm Hg; 0.7 kPa). 1-Methyl-1-[2-(2-propylcarbamoyl-10-phenothiazinyl)propyl]pyrrolidinium bromide, L series (2.05 g), is thereby obtained in the form of a crystalline white solid, m.p. 258° C.

1. customThe suspension obtained
2. filtrationis filtered
3. washthe solid is washed with acetone (3×1 cc)
4. customdried at 40° C. under reduced pressure (5 mm Hg; 0.7 kPa)
5. dissolutionThis amorphous white solid (4.8 g) is dissolved in acetonitrile (12 cc)
6. temperatureunder reflux
7. customThe crystals formed
8. temperatureafter cooling
9. washwashed with ice-cold acetonitrile (3×3 cc)
10. customdried at 40° C. under reduced pressure (5 mm Hg; 0.7 kPa)