反应详情

温度

70 °C

A mixture of 43.9 parts of 1-(4-chloro-1-oxobutyl)pyrrolidine, 55.1 parts of cis-3-methoxy-N-(phenylmethyl)-4-piperidinamine, 37.8 parts of N,N-diethylethanamine and 900 parts of N,N-dimethylformamide was stirred overnight at 70° C. Another portion of 4.4 parts of 1(4-chloro-1-oxobutyl)pyrrolidine was added and stirring was continued overnight at 70° C. The reaction mixture was evaporated and the residue was taken up in a mixture of water and sodium carbonate. The product was extracted with dichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 53.1 parts (59.0%) of cis-1-[4-[3-methoxy-4-[(phenylmethyl)amino]-1-piperidinyl]-1-oxobutyl]pyrrolidine as a residue (int. 42).

1. stirringstirring
2. waitwas continued overnight at 70° C
3. customThe reaction mixture was evaporated
4. additionthe residue was taken up in a mixture of water and sodium carbonate
5. extractionThe product was extracted with dichloromethane
6. washThe extract was washed with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. customThe residue was purified by column chromatography over silica gel using
11. additiona mixture of trichloromethane and methanol
12. customThe pure fractions were collected
13. customthe eluent was evaporated