HRID1433193

反应详情

EQUATION

反应方程式

HRID 1433193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction was cooled
  2. custompartitioned between water and EtOAc
  3. washThe organic layers were washed with water and brine
  4. dry with materialdried with Na2SO4
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated
  7. customThe residue was purified by chromatography (silica, hexanes:EtOAc, 4:1)