HRID1971830

反应详情

EQUATION

反应方程式

HRID 1971830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of 1,2-dichloro-4-iodobenzene (5.44 g, 20 mmol) in DMF (60 ml) was added Bu4NCl (5.56 g, 20 mmol), propenol (4.64 g, 80 mmol), Pd(OAc)2 (224 mg, 1 mmol) and NaHCO3 (10.0 g, 120 mmol) successively at room temperature. The mixture was heated at 50° C. for 12 hour. After cooling to the room temperature, the mixture was poured into ice-water, extracted with DCM three times. The combined organic layers were washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography using PE/EA (20/1) as eluent to afford the title compound (2.01 g, yield 49.8%).

WORKUP

后处理

  1. temperatureAfter cooling to the room temperature
  2. extractionextracted with DCM three times
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by column chromatography