HRID653710
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was heated for 27 further hours
- temperatureunder reflux
- concentrationthe reaction mixture was concentrated to dryness
- additionTo the concentrate was added water, which
- customCrystals thus separated
- filtrationwere collected by filtration
- customRecrystallization from methanol afforded colorless needles (8.8 g, 93%), m.p. 203°-204° C.