反应详情

温度

115 °C

A mixture of methyl 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]benzimidazole-7-carboxylate (3.2 g), sodium azide (7.4 g) and ammonium chloride (6.1 g) in DMF (30 ml) was stirred for 4 days at 115° C. To the reaction mixture was added water, which was adjusted to pH 3-4 with 1N-HCl. Resulting crude crystals (1) were purified by column chromatography on silica gel. The crystals thus obtained were recrystallized from ethyl acetate-methanol to afford colorless prisms (2.27 g, 63%), m p. 168-169° C.

1. customResulting crude crystals (1)
2. customwere purified by column chromatography on silica gel
3. customThe crystals thus obtained
4. customwere recrystallized from ethyl acetate-methanol