HRID653710

反应详情

EQUATION

反应方程式

HRID 653710 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]benzimidazole-7-carboxylate (10 g) and NaBH. (2.2 g) in tetrahydrofuran (100 ml) was added dropwise methanol (19 ml) during 80 minutes. The mixture was heated for 27 further hours under reflux, and the reaction mixture was concentrated to dryness. To the concentrate was added water, which was neutralized with conc. HCl. Crystals thus separated were collected by filtration. Recrystallization from methanol afforded colorless needles (8.8 g, 93%), m.p. 203°-204° C.

WORKUP

后处理

  1. temperatureThe mixture was heated for 27 further hours
  2. temperatureunder reflux
  3. concentrationthe reaction mixture was concentrated to dryness
  4. additionTo the concentrate was added water, which
  5. customCrystals thus separated
  6. filtrationwere collected by filtration
  7. customRecrystallization from methanol afforded colorless needles (8.8 g, 93%), m.p. 203°-204° C.