HRID1660803

反应详情

EQUATION

反应方程式

HRID 1660803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-hydroxy-3-nitro-benzoic acid methyl ester (30 g, 152 mmol) in acetone (1000 mL) was charged into a 2 L reactor and treated with K2CO3 (31.5 g, 228 mol) and benzyl bromide (52 g, 36.1 mL, 304 mmol). The mixture was mechanically stirred at heated at reflux for 16 hours under a light argon flux. After cooling to room temperature the solvent was evaporated. The residue was taken up in ethyl acetate/water and the two phases were separated. The aqueous phase was extracted three times with ethyl acetate (total solvent volume: 1.5 L, total water volume 1 L). The combined organic phases were dried over sodium sulfate and evaporated. 4-Benzyloxy-3-nitro-benzoic acid methyl ester thus obtained was used crude in the following reaction.

WORKUP

后处理

  1. temperatureat heated
  2. temperatureat reflux for 16 hours under a light argon flux
  3. customwas evaporated
  4. customthe two phases were separated
  5. extractionThe aqueous phase was extracted three times with ethyl acetate (total solvent volume: 1.5 L, total water volume 1 L)
  6. dry with materialThe combined organic phases were dried over sodium sulfate
  7. customevaporated