HRID333220

反应详情

EQUATION

反应方程式

HRID 333220 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-fluoro-2-iodo-6-methylbenzoate (440 mg, 1.49 mmol) and copper(I) cyanide (200 mg, 2.24 mmol) were dissolved in N,N-dimethylformamide (5.5 mL) and the resulted solution was refluxed under nitrogen atmosphere for 3 hours. The solvent was removed under reduced pressure and the residue was diluted with dichloromethane and washed with 15% ammonium hydroxide. Organic phase was dried over sodium sulfate, filtered and evaporated. Column chromatography (n-hexane/ethyl acetate: 7/3) afforded title compound (210 mg, 73% yield).

WORKUP

后处理

  1. temperaturethe resulted solution was refluxed under nitrogen atmosphere for 3 hours
  2. customThe solvent was removed under reduced pressure
  3. additionthe residue was diluted with dichloromethane
  4. washwashed with 15% ammonium hydroxide
  5. dry with materialOrganic phase was dried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated