HRID1658244

反应详情

EQUATION

反应方程式

HRID 1658244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-hydroxymethyl-5-nitro-N,N-dimethylbenzamide (17 g.) in glacial acetic acid (340 ml.) was added chromium trioxide (17 g.) in water (17 ml.) and glacial acetic acid (340-1). The reaction mixture was stirred at room temperature for 5 minutes, and then poured into ice-water (2 liters). The aqueous was extracted with chloroform (3 × 500 ml.). The chloroform extracts were combined and neutralised by washing with 10% sodium bicarbonate solution. The chloroform exracts were then washed thoroughly with water and dried over magnesium sulphate. The solution was then filtered and the solvent evaporated off to yeild a gum.

WORKUP

后处理

  1. extractionThe aqueous was extracted with chloroform (3 × 500 ml.)
  2. washby washing with 10% sodium bicarbonate solution
  3. washThe chloroform exracts were then washed thoroughly with water
  4. dry with materialdried over magnesium sulphate
  5. filtrationThe solution was then filtered
  6. customthe solvent evaporated off