HRID1502020
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3-Ethenyl-6-fluoro-2-methoxybenzonitrile (1.67 g, 9.43 mmol) was added to DCM (50 mL) at 0° C. then mCPBA (4.88 g, 28.3 mmol) was added and the reaction mixture was stirred at RT for 16 h. The reaction mixture was washed with saturated aqueous Na2S2O3, then with 1N NaOH followed by brine. The organic layer was separated and dried over Na2SO4, filtered, and evaporated to dryness. The crude product was purified by chromatography through a 120 g. Redi-sep column and eluting with a 0-100% EtOAc/hexane solvent system. Isolated pure 6-fluoro-2-methoxy-3-(oxiran-2-yl)benzonitrile.
WORKUP
后处理
- washThe reaction mixture was washed with saturated aqueous Na2S2O3
- customThe organic layer was separated
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated to dryness
- customThe crude product was purified by chromatography through a 120 g
- washRedi-sep column and eluting with a 0-100% EtOAc/hexane solvent system