HRID1295711
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customat 60° C.
- customovernight
- washthe resulting solution was washed several times with water
- dry with materialThe organic layer was dried (Na2SO4)
- concentrationconcentrated carefully in vacuo at 30° C.
- customto furnish