HRID928946

反应详情

EQUATION

反应方程式

HRID 928946 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Sodium carbonate (19.50 g, 183.96 mmol) was dispersed into a solution of 2,3,4-trifluorophenol (13.64 g, 92.10 mmol) in acetone (300 mL). To the stirred suspension was added benzyl bromide (17.31 g, 101.21 mmol) dropwisely. The mixture was heated under reflux at 50° C. for 24 h. The acetone was removed under reduced pressure and the residue was dissolved in water (300 mL). The solution was extracted with ethyl acetate (100 mL×2). The combined organic extracts were washed with 5% sodium hydroxide (100 mL) and brine (100 mL) sequentially and dried over Na2SO4. The solvent was removed in vacuo to yield a pale yellow solid (19.89 g, 90.7% yield). 1H NMR (400 MHz, CDCl3): δ 7.40 (m, 5H), 6.85 (m, 1H), 6.64 (m, 1H), 5.15 (s, 2H).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. customThe acetone was removed under reduced pressure
  3. dissolutionthe residue was dissolved in water (300 mL)
  4. extractionThe solution was extracted with ethyl acetate (100 mL×2)
  5. washThe combined organic extracts were washed with 5% sodium hydroxide (100 mL) and brine (100 mL) sequentially
  6. dry with materialdried over Na2SO4
  7. customThe solvent was removed in vacuo