反应详情

A mixture of 50 parts of phenyl [4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]carbamate, 22.7 parts of ethyl 2-piperidinecarboxylate, 4 parts of N,N-dimethyl-4-pyridinamine and 300 parts of 1,4-dioxane was stirred for 5 hours at reflux temperature. After saturation with water, the reaction mixture was heated for 30 minutes. After cooling, the precipitated product was filtered off, washed with 2-propanol and purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (99:1 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 1-butanol. The product was filtered off and dried, yielding 24.8 parts (47.5%) of 5,6,7,8-tetrahydro-2-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]imidazo[1,5-a]pyridine-1,3(2H,8aH)-dione; mp. 223.4° C. (int. 17).

1. temperatureat reflux temperature
2. temperatureAfter cooling
3. filtrationthe precipitated product was filtered off
4. washwashed with 2-propanol
5. custompurified by column chromatography over silica gel using
6. additiona mixture of trichloromethane and methanol (99:1 by volume) as eluent
7. customThe pure fractions were collected
8. customthe eluent was evaporated
9. customThe residue was crystallized from 1-butanol
10. filtrationThe product was filtered off
11. customdried