反应详情

A mixture of 70.4 parts of 1-(phenylmethyl)piperazine, 39.4 parts of 1-(2-chloroethyl)-1,3-dihydro-2H-benzimidazol-2-one and 360 parts of methylbenzene is stirred and refluxed overnight. The reaction mixture is cooled, water is added and the layers are separated. The methylbenzene-phase is washed three times with water, dried, filtered and evaporated. The solid residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is boiled in 2,2'-oxybispropane. The whole is cooled on an ice-bath. The product is filtered off and crystallized from a mixture of 2,2'-oxybispropane and a small amount of 2-propanol, yielding 1,3-dihydro-1-{2-[4-(phenylmethyl)-1-piperazinyl]ethyl}-2H-benzimidazol-2-one; mp. 136.5° C.

1. temperaturerefluxed overnight
2. temperatureThe reaction mixture is cooled
3. customthe layers are separated
4. washThe methylbenzene-phase is washed three times with water
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe solid residue is purified by column-chromatography over silica gel using
9. additiona mixture of trichloromethane and methanol (95:5) as eluent
10. customThe pure fractions are collected
11. customthe eluent is evaporated
12. temperatureThe whole is cooled on an ice-bath
13. filtrationThe product is filtered off
14. customcrystallized from a mixture of 2,2'-oxybispropane