反应详情

A mixture of 4.5 parts of 7-(3-chloropropyl)-3,7-dihydro-1,3-dimethyl-1H-purine-2,6-dione monohydrochloride, 3 parts of 3-(4-piperidinyl)-1H-indol, 8 parts of sodium carbonate, 0.1 parts of sodium iodide and 240 parts of 4-methyl-2-pentanone was stirred and refluxed for 20 hours. The whole was filtered while hot and the filtrate was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (92:8 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was converted into the (E)-2-butenedioate salt in 2-propanol. The salt was filtered off and dried, yielding 3.9 parts (48%) of 3,7-dihydro-7-[3-[4-(1H-indol-3-yl)-1-piperidinyl]propyl]-1,3-dimethyl-1H-purine-2,6-dione (E)-2-butenedioate(1:1); mp. 222.7° C. (compound 13).

1. temperaturerefluxed for 20 hours
2. filtrationThe whole was filtered while hot and the filtrate
3. customwas evaporated
4. customThe residue was purified by column chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol (92:8 by volume) as eluent
6. customThe pure fractions were collected
7. customthe eluent was evaporated
8. filtrationThe salt was filtered off
9. customdried