反应详情

温度

70 °C

A mixture of 5.55 parts of N-(dihydro-3,3-diphenyl-2(3H)-furanylidene)-N-methylmethanaminium bromide, 4.85 parts of 1-[(4-fluorophenyl)methyl]-2-(4-piperidinylmethyl)-1H-benzimidazole, 2 parts of sodium carbonate and 90 parts of N,N-dimethylformamide was stirred overnight at 70° C. The reaction mixture was poured into water. The product was extracted with 4-methyl-2-pentanone. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 1.8 parts (20%) of 4-[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]methyl]-N,N-dimethyl-α,α-diphenyl-1-piperidinebutanamide; mp. 151.4° C. (150).

1. extractionThe product was extracted with 4-methyl-2-pentanone
2. customThe extract was dried
3. filtrationfiltered
4. customevaporated
5. customThe residue was purified by column chromatography over silica gel using
6. additiona mixture of trichloromethane and methanol
7. customThe pure fractions were collected
8. customthe eluent was evaporated
9. customThe residue was crystallized from acetonitrile
10. filtrationThe product was filtered off
11. customdried