反应详情

3.9 g 1-(Piperidin-4-yl)-5-fluoro-2-pentafluoroethyl-1H-benzoimidazole, 4.4 g 1-(3-bromo-propylsulfanyl)-4-fluoro-benzene and 2 g K2CO3 were stirred in 50 ml DMF at 100° C. for 2 h. After cooling the mixture was poured into water and was extracted 2× with ethyl acetate. The organic layer was tracted 3× with water, dried and evaporated. The resulting oil was purified by flash chromatography with dichloromethane, the purified fractions were dissolved in acetone after evaporation of the solvent, and the solution was acidified with etherical HCl. After evaporation of the solvent the resulting crystals were filtered with diisopropyl ether. The crystals were dissolved in acetone again and evaporated to a volume of 2 ml. The product crystallized as hydrochloride to give 0.5 g product (mp. 208–209° C.).

1. temperatureAfter cooling the mixture
2. extractionwas extracted 2× with ethyl acetate
3. customdried
4. customevaporated
5. customThe resulting oil was purified by flash chromatography with dichloromethane
6. dissolutionthe purified fractions were dissolved in acetone
7. customafter evaporation of the solvent
8. customAfter evaporation of the solvent the resulting crystals
9. filtrationwere filtered with diisopropyl ether
10. dissolutionThe crystals were dissolved in acetone again
11. customevaporated to a volume of 2 ml
12. customThe product crystallized as hydrochloride