HRID1519589
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A solution of 4-(2,3-dihydroxypropyl)-2,6-difluorobenzonitrile (500 mg, 2.4 mmol) in 10 mL of methanol and 3 mL of water was cooled to 0° C. by ice bath, then NaIO4 (754 mg, 3.5 mmol) was added and the mixture was stirred at 0° C. for two hours. The reaction was monitored according to TLC. The mixture was filtered and concentrated. The residue was dissolved in DCM, dried over anhydrous sodium sulfate, and then purified by flash column chromatography to give 2,6-difluoro-4-(2-oxoethyl)benzonitrile. MS m/z: 182 (M+1)+.
WORKUP
后处理
- filtrationThe mixture was filtered
- concentrationconcentrated
- dissolutionThe residue was dissolved in DCM
- dry with materialdried over anhydrous sodium sulfate
- custompurified by flash column chromatography