HRID1475777

反应详情

EQUATION

反应方程式

HRID 1475777 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3.9 g of 3-fluoro-4-hydroxy-benzoic acid methyl ester were dissolved using 25 ml of acetic acid and 25 ml of DCM. The mixture was cooled to 0° C. and 1.4 ml bromine added slowly (30 minutes) at 0° C. Stirring was continued at room temperature for 18 h. Then, 200 ml of EA and a solution of 7.6 g Na2SO3 in 50 ml of water were added and the resulting mixture was stirred for 10 minutes at room temperature. The layers were separated, and the organic layer was washed using first 50 ml of water and second 50 ml of a saturated aqueous NaCl-solution. The organic layer was dried using MgSO4 and evaporated to yield 5.0 g of the title compound that was used without further purification.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred for 10 minutes at room temperature
  2. customThe layers were separated
  3. washthe organic layer was washed
  4. customThe organic layer was dried
  5. customevaporated