反应详情

温度

70 °C

A mixture of 3.47 parts of 4-chloro-1-(3-pyridinyl)-1-butanone, 4.5 parts of cis-4-amino-5-chloro-2-methoxy-N-(3-methoxy-4-piperidinyl)benzamide, 1.94 parts of N,N-diethylethanamine, 0.1 parts of potassium iodide and 67.5 parts of N,N-dimethylformamide was stirred and heated for 48 hours at 70° C. The reaction mixture was evaporated. The residue was washed with a sodium carbonate solution in water and purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 1.36 parts (20%) of cis-4-amino-5-chloro-2-methoxy-N-[3-methoxy-1-[4-oxo-4-(3-pyridinyl)butyl]-4-piperidinyl]benzamide; mp. 166.2° C. (compound 1).

1. customThe reaction mixture was evaporated
2. washThe residue was washed with a sodium carbonate solution in water
3. custompurified by column chromatography over silica gel using
4. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
5. customThe pure fractions were collected
6. customthe eluent was evaporated
7. customThe residue was crystallized from acetonitrile
8. filtrationThe product was filtered off
9. customdried