反应详情

温度

120 °C

A mixture of 9.8 parts of ethyl 4-amino-1-piperidinecarboxylate and 15 parts of 2-chloro-1-(4-fluorophenylmethyl)-1H-benzimidazole was heated to 120° C. The mixture was stirred at 120° C. during 43 hours. After cooling, 100 parts of trichloromethane were added and the whole was thouroughly stirred. The mixture was washed with water. The aqueous layer was separated and the organic mixture was filtered and evaporated. The collected solid material was dissolved in 100 parts of water and subsequently 100 parts of 20% sodium hydroxide solution were added. The precipitate was filtered and dried in vacuo at 50° C., yielding 12.1 parts (40.5%) of ethyl 4-[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]amino]-1-piperidinecarboxylate; mp. 181° C. (compound 21).

1. temperatureAfter cooling
2. stirringthe whole was thouroughly stirred
3. washThe mixture was washed with water
4. customThe aqueous layer was separated
5. filtrationthe organic mixture was filtered
6. customevaporated
7. dissolutionThe collected solid material was dissolved in 100 parts of water and subsequently 100 parts of 20% sodium hydroxide solution
8. additionwere added
9. filtrationThe precipitate was filtered
10. customdried in vacuo at 50° C.