反应详情

A mixture of methyl 1-[(2'-cyanobiphenyl-4-yl)methyl]-2-oxo-2,3-dihydrobenzimidazole-7-carboxylate (8.02 g) in phosphorus oxychloride (30 ml) was heated under reflux for 8 hours. The reaction mixture was concentrated and the resulting residue was poured into ice-water. The mixture was extracted with chloroform. The extract was washed with water, dried and evaporated. The residue was purified by column chromatography on silica gel to give crystals, which were recrystallized from chloroform-methanol to afford colorless needles (2.2 g, 28%), m.p. 154°-157° C.

1. temperaturewas heated
2. temperatureunder reflux for 8 hours
3. concentrationThe reaction mixture was concentrated
4. additionthe resulting residue was poured into ice-water
5. extractionThe mixture was extracted with chloroform
6. washThe extract was washed with water
7. customdried
8. customevaporated
9. customThe residue was purified by column chromatography on silica gel
10. customto give crystals, which
11. customwere recrystallized from chloroform-methanol