HRID1270786

反应详情

EQUATION

反应方程式

HRID 1270786 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

5-Methoxy-2-bromophenylacetic acid (56 g, 0.23 mol) is dissolved in CH2Cl2 (350 mL) and a catalytic amount of DMF is added and the solution stirred and cooled to 0° C. Thionyl chloride (41 mL, 0.34 mol) is added dropwise. The reaction mixture is heated at reflux temperature overnight and then cooled to room temperature. Solvents are removed by rotary evaporator. Twice benzene (500 mL) is added to the residual oil and the benzene solution is evaporated by rotary evaporator to remove any additional volatile components. The residual oil is crystallized from hexanes to give 5-methoxy-2-bromophenylacetyl chloride.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux temperature overnight
  3. temperaturecooled to room temperature
  4. customSolvents are removed by rotary evaporator
  5. additionTwice benzene (500 mL) is added to the residual oil
  6. customthe benzene solution is evaporated by rotary evaporator
  7. customto remove any additional volatile components
  8. customThe residual oil is crystallized from hexanes