反应详情

A mixture of 1.6 parts of 1-(1-chloroethyl)-4-fluorobenzene, 3.2 parts of N-[1-(2-phenylethyl)-4-piperidinyl]-1H-benzimidazol-2-amine, 1 part of sodium carbonate, 0.1 parts of potassium iodide and 120 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. The reaction mixture is cooled, poured onto water and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 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 1.8 parts (40.7%) of 1-[1-(4-fluorophenyl)ethyl]-N-[1-(2-phenylethyl)-4-piperidinyl]-1H-benzimidazol-2-amine; mp. 161.7° C.

1. temperatureThe reaction mixture is cooled
2. additionpoured onto water
3. customthe layers are separated
4. customThe organic phase is dried
5. filtrationfiltered
6. customevaporated
7. customThe residue is purified by column-chromatography over silica gel using
8. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
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