HRID1295711

反应详情

EQUATION

反应方程式

HRID 1295711 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

t-BuOK (3.0 g, 27 mmol) was added to a mixture of 1,2,4,5-tetrafluorobenzene (2.0 g, 13.3 mmol) and ethylene glycol (7.5 mL, 133 mmol) in DMSO (50 mL) and heated at 80° C. for 1 h and then at 60° C. overnight. EtOAc was added and the resulting solution was washed several times with water. The organic layer was dried (Na2SO4) and concentrated carefully in vacuo at 30° C. to furnish 1.5 g (containing ˜14% EtOAc) of the title compound as a white semisolid. NMR analysis supports the stated structure. This material was used directly in the next step.

WORKUP

后处理

  1. customat 60° C.
  2. customovernight
  3. washthe resulting solution was washed several times with water
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. concentrationconcentrated carefully in vacuo at 30° C.
  6. customto furnish