HRID1433193
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
- 100 °C
PROCEDURE
实验过程
A mixture of 4-trifluoromethyl-phenol (25.0 g, 0.154 mol), bromoacetonitrile (12.9 mL, 0.185 mol), sodium carbonate (32.7 g, 0.308 mol), and sodium iodide (23.1 g, 0.154 mol) in 214 mL of DMF was heated at 100° C. for 2 hours. The reaction was cooled, and partitioned between water and EtOAc. The organic layers were washed with water and brine, dried with Na2SO4, filtered and the filtrate was concentrated. The residue was purified by chromatography (silica, hexanes:EtOAc, 4:1) to afford the title compound as a colorless oil (29.8 g, 96%). 1H NMR (400 MHz, CD3Cl) δ (ppm): 7.63 (d, 2H), 7.07 (d, 2H), 4.83 (s, 2H).
WORKUP
后处理
- temperatureThe reaction was cooled
- custompartitioned between water and EtOAc
- washThe organic layers were washed with water and brine
- dry with materialdried with Na2SO4
- filtrationfiltered
- concentrationthe filtrate was concentrated
- customThe residue was purified by chromatography (silica, hexanes:EtOAc, 4:1)