反应详情

温度

100 °C

To a stirred mixture of 13.2 parts of 2-methyl-1H-benzimidazole, 3 parts of N,N,N-triethylbenzenemethanaminium chloride and 225 parts of a sodium hydroxide solution 60% are added 25 parts of 1,4-dichlorobutane. The whole is heated to about 100° C. and stirring is continued for one hour at this temperature. The reaction mixture is cooled and poured onto ice-water. The product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (90:10) as eluent. The pure fractions are collected and eluent is evaporated, yielding 1-(4-chlorobutyl)-2-methyl-1H-benzimidazole as a residue.

1. temperatureThe reaction mixture is cooled
2. additionpoured onto ice-water
3. extractionThe product is extracted with methylbenzene
4. customThe extract 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 (90:10) as eluent
9. customThe pure fractions are collected
10. customeluent is evaporated