HRID636503

反应详情

EQUATION

反应方程式

HRID 636503 的结构方程式

PROCEDURE

实验过程

A mixture of 3-benzyloxy-2-amino-N-methylaniline (600 mg), isobutyric acid (243 mg) and 4N hydrochloric acid (3.5 ml) was refluxed for 3 hours, and the solvent was removed in vacuo. Chloroform and saturated sodium bicarbonate solution were added to the residue. The separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by silica gel column chromatogrpahy (chloroform:methanol=50:1, v/v) to give 4-hydroxy-2-isopropyl-1-methyl-1H-benzimidazole (33 mg).

WORKUP

后处理

  1. temperaturewas refluxed for 3 hours
  2. customthe solvent was removed in vacuo
  3. additionChloroform and saturated sodium bicarbonate solution were added to the residue
  4. washThe separated organic layer was washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by silica gel column chromatogrpahy (chloroform