反应详情

温度

20 °C

A boiling solution of N-cyclobutylmethyl-10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide, L series (1.7 g) in 2-propanol (17 cc) containing fumaric acid (0.47 g) is allowed to cool. The mixture is concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C. to give a residue which is taken up in isopropyl ether (100 cc). The mixture is stirred for 1 hour at 20° C. The suspension obtained is filtered and the solid is washed with isopropyl ether (2×5 cc) and dried under reduced pressure (5 mm Hg; 0.67 kPa) at 50° C. to give a cream-coloured powder, which is dissolved in acetone (25 cc) under reflux. Crystallization develops. The mixture is stirred for 16 hours at 20° C. and the crystals are drained and dried under reduced pressure (5 mm Hg; 0.67 kPa) at 50° C. N-Cyclobutylmethyl-10-[1-(1-pyrrolidinyl)-2-propyl]-2-phenothiazinecarboxamide fumarate, L series (0.64 g) is thereby obtained in the form of cream-coloured crystals, m.p., 126°-128° C.

1. temperatureto cool
2. concentrationThe mixture is concentrated under reduced pressure (30 mm Hg; 4 kPa) at 40° C.
3. customto give a residue which
4. customThe suspension obtained
5. filtrationis filtered
6. washthe solid is washed with isopropyl ether (2×5 cc)
7. customdried under reduced pressure (5 mm Hg; 0.67 kPa) at 50° C.
8. customto give a cream-coloured powder, which
9. temperatureunder reflux
10. customCrystallization
11. stirringThe mixture is stirred for 16 hours at 20° C.
12. customdried under reduced pressure (5 mm Hg; 0.67 kPa) at 50° C