HRID487192

反应详情

EQUATION

反应方程式

HRID 487192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2-n-butyl-1-(2-chlorophenyl)methyl-6-hydroxymethyl-1H-benzimidazole (1 g, 3.04 mmol, prepared in Example 9(i)), toluene (500 mL) and activated manganese dioxide (4 g) was refluxed with a Dean-Stark water separator for 4 hours. The mixture was filtered hot, concentrated and the crude product was treated with celite in methylene chloride to afford, after concentration, a residue that crystallized. Recrystallization from hexane gave 0.65 g (66%) of 2-n-butyl-1-{(2-chlorophenyl)methyl}-1H-benzimidazole-7-carboxaldehyde; mp 113.5°-115° C.

WORKUP

后处理

  1. filtrationThe mixture was filtered hot
  2. concentrationconcentrated
  3. additionthe crude product was treated with celite in methylene chloride
  4. customto afford
  5. concentrationafter concentration
  6. customa residue that crystallized
  7. customRecrystallization from hexane