反应详情

A mixture of 12 parts of ethyl 4-[5-(4-fluorophenyl)-5-(3-pyridinyl)pentyl]-2-methyl-1-piperazinecarboxylate, 16 parts of potassium hydroxide and 128 parts of 2-propanol was stirred for 4 days at reflux temperature. After cooling, the reaction mixture was evaporated. Water was added to the residue and the mixture was evaporated till all traces of 2-propanol were removed (this was repeated twice). The residue was taken up in water and the product was extracted with dichlormethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichlormethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 6.7 parts (67.6%) of 1-[5-(4-fluorophenyl)-5-(3-pyridinyl)pentyl]-3-methylpiperazine as a residue (int. 39).

1. temperatureat reflux temperature
2. temperatureAfter cooling
3. customthe reaction mixture was evaporated
4. additionWater was added to the residue
5. customthe mixture was evaporated till all traces of 2-propanol
6. customwere removed (
7. extractionthe product was extracted with dichlormethane
8. washThe extract was washed with water
9. customdried
10. filtrationfiltered
11. customevaporated
12. customThe residue was purified by column chromatography over silica gel using
13. additiona mixture of trichlormethane and methanol
14. customThe pure fractions were collected
15. customthe eluent was evaporated