HRID890372

反应详情

EQUATION

反应方程式

HRID 890372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-fluorophenylacetic acid (1 equivalent) was dissolved in dichloroethane (1.3 M) containing SOCl2 (3 equivalents), the mixture was refluxed for 90 minutes and the solvent was removed. Solution of this crude product in CH2Cl2 was added dropwise within 60 minutes to AlCl3 (2 eq) in CH2Cl2 (0.4 M) while stirring at 0° C. Thereafter, ethylene was introduced at 0° C. over 45 minutes, whereupon the mixture was stirred further at room temperature for 1 hour, and thereafter was treated at 0° C. with ice-water. The organic phase was washed with 1 N HCl (2×), NaHCO3 (sat. sol.), dried and evaporated. The residue was triturated with hexane, yielding the product as a bright yellow solid.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 90 minutes
  2. customthe solvent was removed
  3. stirringwas stirred further at room temperature for 1 hour
  4. washThe organic phase was washed with 1 N HCl (2×), NaHCO3 (sat. sol.)
  5. customdried
  6. customevaporated
  7. customThe residue was triturated with hexane