HRID1267886

反应详情

EQUATION

反应方程式

HRID 1267886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

1-(Vinyloxy)-2-iodo-4-(trifluoromethoxy)benzene (Description 11; 7.6 g, 23 mmol) and chloroiodomethane (5.4 mL, 74 mmol) were dissolved in 1,2-dichloroethane (40 mL) and cooled to 0° C. Diethyl zinc (3.8 mL, 36.8 mmol) was then added dropwise. The solution was allowed to warm to room temperature for 10 minutes, then cooled back to 0° C. when it was quenched with saturated aqueous ammonium chloride solution (50 mL). The suspension formed was extracted with 50% diethyl ether/hexane (2×100 mL) and the extracts dried (MgSO4). Concentration yielded a yellow oil which was purified by silica chromatography to give the title compound as a clear oil (5.84 g, 17 mmol).

WORKUP

后处理

  1. temperatureto warm to room temperature for 10 minutes
  2. temperaturecooled back to 0° C. when it
  3. customwas quenched with saturated aqueous ammonium chloride solution (50 mL)
  4. customThe suspension formed
  5. extractionwas extracted with 50% diethyl ether/hexane (2×100 mL)
  6. dry with materialthe extracts dried (MgSO4)
  7. concentrationConcentration
  8. customyielded a yellow oil which
  9. customwas purified by silica chromatography