HRID333220
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe resulted solution was refluxed under nitrogen atmosphere for 3 hours
- customThe solvent was removed under reduced pressure
- additionthe residue was diluted with dichloromethane
- washwashed with 15% ammonium hydroxide
- dry with materialOrganic phase was dried over sodium sulfate
- filtrationfiltered
- customevaporated