反应详情

温度

60 °C

To a THF solution (40 mL) of (4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone (3.0 g, 9.0 mmol) were added THF (40 mL) and fumaric acid (3.3 g, 28.4 mmol). The resulting mixture was heated to 60° C. and stirred for 0.5 h. The resulting suspension was cooled to 0° C. and the resulting precipitate was collected by filtration, washed with THF (20 mL), and dried in a vacuum oven at 65° C. for 20 h to yield crude title compound as a white solid. A suspension of crude (4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl-phenyl)-methanone, mono-fumarate (5.7 g, 12.7 mmol) in absolute EtOH (110 mL) was heated to 70° C. Any insoluble material was removed by filtration through a Celite pad. The filtrate was reheated to 65° C. and then cooled to 0° C. The precipitate was collected by filtration and washed with MTBE (20 mL). The solids were dried in a vacuum oven at 65° C. for 20 h to yield the title compound as a white solid.

1. temperatureThe resulting suspension was cooled to 0° C.
2. filtrationthe resulting precipitate was collected by filtration
3. washwashed with THF (20 mL)
4. customdried in a vacuum oven at 65° C. for 20 h
5. customto yield crude title compound as a white solid
6. temperaturewas heated to 70° C
7. customAny insoluble material was removed by filtration through a Celite pad
8. customwas reheated to 65° C.
9. temperaturecooled to 0° C
10. filtrationThe precipitate was collected by filtration
11. washwashed with MTBE (20 mL)
12. customThe solids were dried in a vacuum oven at 65° C. for 20 h