HRID1161184

反应详情

EQUATION

反应方程式

HRID 1161184 的结构方程式

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

A round bottom flask was charged with 4-chloro-2-methyl-3-nitrobenzoic acid (11.00 g, 0.05102 mol) and methanol (110 mL, 2.7 mol) and thionyl chloride (4.5 mL, 0.061 mol) was added at 0° C. and the reaction heated at 75° C. for 3 hours. The solvent was removed under reduced pressure and the residue dissolved in ethyl acetate (300 mL) and washed with aqueous sodium bicarbonate, water and brine. The organic extracts were dried over sodium sulfate and the solvent removed to recover the esters. MS m/z=230.3 (M+H).

WORKUP

后处理

  1. additionwas added at 0° C.
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue dissolved in ethyl acetate (300 mL)
  4. washwashed with aqueous sodium bicarbonate, water and brine
  5. dry with materialThe organic extracts were dried over sodium sulfate
  6. customthe solvent removed
  7. customto recover the esters