反应详情

A mixture of 169.8 parts of 1,1'-(4-chlorobutylidene)bis[4-fluorobenzene], 93.5 parts of hexahydro-3,3-dimethylimidazo[1,5-a]pyrazin-1(5H)-one, 128.3 parts of sodium carbonate, 0.1 parts of potassium iodide and 1200 parts of 4-methyl-2-pentanone was stirred and refluxed for 8 hours using a water-separator. After cooling overnight to room temperature, the reaction mixture was filtered. The filtrate was evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was triturated in 2,2'-oxybispropane. The product was filtered off and dried, yielding 108 parts of 7-[4,4-bis(4-fluorophenyl)butyl]hexahydro-3,3-dimethylimidazo[1,5-a]pyrazin-1(5H)-one; mp. 148.4° C. (intermediate 90).

1. temperaturerefluxed for 8 hours
2. temperatureAfter cooling overnight to room temperature
3. filtrationthe reaction mixture was filtered
4. customThe filtrate was evaporated
5. customThe residue was purified by column-chromatography over silica gel using
6. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
7. customThe pure fractions were collected
8. customthe eluent was evaporated
9. customThe residue was triturated in 2,2'-oxybispropane
10. filtrationThe product was filtered off
11. customdried