反应详情

温度

60 °C

A mixture of 2.8 parts of 3-(chloromethyl)pyridine hydrochloride, 4.7 parts of cis-4-amino-5-chloro-2-methoxy-N-(3-methoxy-4piperidinyl)benzamide, 5.3 parts of sodium carbonate and 68 of N,N-dimethylformamide was stirred for 5 hours at about 60° C. The reaction mixture was cooled to room temperature and filtered. The filtrate was evaporated. The solid residue was 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 eluent was evaporated. The residue was crystallized from ethanol. The product was filtered off and dried, yielding 3.84 parts (64.2%) of cis-4-amino-5-chloro-2-methoxy-N-[3-methoxy-1-(3-pyridinylmethyl)-4-piperidinyl]benzamide; mp. 188.9° C. (compound 91).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered
3. customThe filtrate was evaporated
4. customThe solid residue was purified by column-chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
6. customThe pure fractions were collected
7. customeluent was evaporated
8. customThe residue was crystallized from ethanol
9. filtrationThe product was filtered off
10. customdried