反应详情

温度

5 °C

The free duloxetine (3 g) was first dissolved in dichloromethane (5 ml), then an ethanol solution (2 ml) containing 20% HCl was added at 0° C. with stirring, followed by hexane (40 ml). The crystalline product came out after the solution was cooled at 0-10° C. for 10 hours. The product was collected by filtration, washed with hexane and dried (1.8 g, 55% yield, m.p. 148-154° C.). Its purity was 98.4% with an optical purity of 99.6%. The DTA result shown m.p. was 160.6° C. The crystalline form, designated as Form III, was thus obtained.

1. additionwas added at 0° C.
2. filtrationThe product was collected by filtration
3. washwashed with hexane
4. customdried (1.8 g, 55% yield, m.p. 148-154° C.)
5. customThe DTA result
6. customwas thus obtained