HRID1681365

反应详情

EQUATION

反应方程式

HRID 1681365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Bis(4-fluorophenyl)methanol was refluxed in toluene with an equimolar amount of bromoethanol in presence of a catalytic amount of p-toluenesulphonic acid. The mixture was refluxed for 12 hrs. in a Dean-Stark apparatus. The solvent was evaporated and the residue was dissolved in ether, washed with water (three times) and brine (three times). The organic layer was dried with sodium sulfate, filtered, concentrated and the residue was purified by distillation to obtain in 80% yield 1-bromo-2-[bis(4-fluorophenyl)methoxy]ethane, b.p. 170° C. at 0.1 mm Hg.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 12 hrs
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in ether
  4. washwashed with water (three times) and brine (three times)
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. distillationthe residue was purified by distillation