HRID220853

反应详情

EQUATION

反应方程式

HRID 220853 的结构方程式

PROCEDURE

实验过程

A solution of 2-chloro-4-hydroxy-benzoic acid (3.70 g, 21.4 mmol)) in methanol (50 ml) was treated with thionyl chloride (2.4 ml, 32 mmol) dropwise and stirred for 24 hours and the solvents were removed in vacuo. The residue was dissolved in ethyl acetate and washed with sat. sodium hydrogen carbonate, dried and solvents were removed in vacuo. The residue was purified by column chromatography on silica gel (eluant with 30% EtOAc:70% cyclohexane) to yield the desired product as a yellow solid, 3.68 g, 92%.

WORKUP

后处理

  1. customthe solvents were removed in vacuo
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with sat. sodium hydrogen carbonate
  4. customdried
  5. customsolvents were removed in vacuo
  6. customThe residue was purified by column chromatography on silica gel (eluant with 30% EtOAc:70% cyclohexane)