HRID62788

反应详情

EQUATION

反应方程式

HRID 62788 的结构方程式

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To (4-cyclopentyl-3-(trifluoromethyl)phenyl)methanol (1.21 g, 4.95 mmol) was added thionyl chloride (5.5 mL, 74.2 mmol). The mixture was heated at 50° C. for 2 h before it was allowed to cool to room temperature and stirred at room temperature overnight. The mixture was poured into ice and stirred for 5 min before it was extracted with dichloromethane. The organic extract was washed with saturated aqueous sodium bicarbonate solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give the title compound as an oil (1.16 g). 1H NMR (400 MHz, CDCl3) δ ppm 1.55-1.63 (m, 2H), 1.69-1.77 (m, 2H), 1.82-1.90 (m, 2H), 2.05-2.13 (m, 2H), 3.37 (quintet, J=8.59 Hz, 1H), 4.58 (s, 2H), 7.46 (d, J=8.00 Hz, 1H), 7.52 (d, J=8.00 Hz, 1H), 7.61 (d, J=1.52 Hz, 1H).

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. additionThe mixture was poured into ice
  3. stirringstirred for 5 min before it
  4. extractionwas extracted with dichloromethane
  5. extractionThe organic extract
  6. washwas washed with saturated aqueous sodium bicarbonate solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure