HRID1980229

反应详情

EQUATION

反应方程式

HRID 1980229 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

8 g. (0.05 moles) of α-cyano-phenylacetic acid are dissolved in 80 ml. of dichloromethane. 10.2 g. (0.05 moles) of phosphorus pentachloride are added and the mixture is stirred for two hours at the boiling point of dichloromethane. The solvent is distilled off and the residue is taken up in carbontetrachloride and the solution is added dropwise to 9.2 g. (0.05 moles) of pentafluorophenol and 4 ml. (0.05 moles) of pyridine-dissolved in 200 ml. of carbontetrachloride. The reaction mixture is cooled to 0° C. and the pyridine chlorohydrate is washed with 2n hydrochloride acid. The organic layer is washed twice with 40 ml. of water, dried over magnesium sulfate and evaporated. The α-cyano-phenylacetic acid-pentafluorophenyl ester is recrystallized from petrolether

WORKUP

后处理

  1. distillationThe solvent is distilled off
  2. additionthe solution is added dropwise to 9.2 g
  3. washthe pyridine chlorohydrate is washed with 2n hydrochloride acid
  4. washThe organic layer is washed twice with 40 ml
  5. dry with materialof water, dried over magnesium sulfate
  6. customevaporated
  7. customThe α-cyano-phenylacetic acid-pentafluorophenyl ester is recrystallized from petrolether