反应详情

A 2-L Erlenmeyer flask was charged with 205.5 g of 3-[8-[4-(2,2-diphenylethenyl)-1-piperidinyl]octyl]pyridine 420 mL of 2B ethanol, and 55.5 g (5% excess) of fumaric acid. The mixture was heated on a steam cone to solution and filtered through Celite into a 12-L flask equipped with a mechanical stirrer. The filter cake was washed with an additional 420 mL of warm 2B ethanol. The stirred filtrate was diluted rapidly with 5.10 L of acetone. Crystallization began within a few minutes. The suspension was cooled in an ice-acetone bath for 1.0 hour and filtered. The solid was washed with 2×1.0 L=2.0 L of cold acetone and dried in a forced air oven at 75° to give 249.9 g (97% yield) of 3-[8-[4-(2,2-diphenylethenyl)-1-piperidinyl]octyl]pyridine (E)-2-butenedioate salt as a white solid, mp 126°-127°. Lc showed this material to be homogeneous.

1. temperatureThe mixture was heated on a steam cone to solution
2. filtrationfiltered through Celite into a 12-L flask
3. customequipped with a mechanical stirrer
4. washThe filter cake was washed with an additional 420 mL
5. temperatureof warm 2B ethanol
6. additionThe stirred filtrate was diluted rapidly with 5.10 L of acetone
7. customCrystallization
8. waitbegan within a few minutes
9. temperatureThe suspension was cooled in an ice-acetone bath for 1.0 hour
10. filtrationfiltered
11. washThe solid was washed with 2×1.0 L=2.0 L of cold acetone
12. customdried in a forced air oven at 75°