反应详情

温度

190 °C

A mixture of 5.4 parts of urea and 13.7 parts of N1 -{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-4-(trifluoromethyl)-1,2-benzenediamine is stirred and heated for 4 hours at 190° C. The reaction mixture is cooled to room temperature and diluted with water. After the addition of trichloromethane, the layers are separated. The aqueous phase is extracted with trichloromethane. The combined organic phases are washed with water, dried, filtered and evaporated. The oily residue is purified by column-chromatography over silica gel using trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 1-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1,3-dihydro-5-(trifluoromethyl)-2H-benzimidazol-2-one; mp. 152.7° C.

1. temperatureThe reaction mixture is cooled to room temperature
2. customthe layers are separated
3. extractionThe aqueous phase is extracted with trichloromethane
4. washThe combined organic phases are washed with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe oily residue is purified by column-chromatography over silica gel
9. customThe pure fractions are collected
10. customthe eluent is evaporated
11. customThe residue is crystallized from 2,2'-oxybispropane
12. filtrationThe product is filtered off
13. customdried