HRID1611744

反应详情

EQUATION

反应方程式

HRID 1611744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

11.9 g of methyl 2,6-dimethylbenzoate are initially charged in 50 ml of chlorobenzene admixed at room temperature with 8.2 g of sulfuryl chloride and 40 mg of AIBN. The mixture is stirred at 60–90° C. for 2 h. Afterwards, the mixture is admixed with 80 ml of saturated NaHCO3 solution. After the phase separation, the organic phase is washed with 100 ml of 10% Na2SO3 solution, the organic phase is dried over magnesium sulfate and the chlorobenzene is distilled off in vacuo. 15.5 g of colorless liquid are obtained. The product is distilled under high vacuum (0.1 mbar, 66–77° C.). Yield: 10.2 g (71% of theory; 95.2 area %).

WORKUP

后处理

  1. customAfter the phase separation
  2. washthe organic phase is washed with 100 ml of 10% Na2SO3 solution
  3. dry with materialthe organic phase is dried over magnesium sulfate
  4. distillationthe chlorobenzene is distilled off in vacuo