HRID516274

反应详情

EQUATION

反应方程式

HRID 516274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To an aqueous (400 ml) solution of 4-bromo-2,3-difluorophenol (T-1) (195.0 g), bromoethane (196.2 g) and tetrabutylammonium bromide (hereinafter, abbreviated as TBAB) (24.2 g), sodium hydroxide (75.9 g) was added, and heating agitation was carried out at 80° C. for 6 hours in a nitrogen atmosphere. After completion of the reaction, extraction was carried out with heptane, an organic layer was washed with water and a saturated aqueous solution of sodium chloride, and then the resultant solution was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and thus a black oily matter was obtained. The resultant material was purified by distillation, and thus 1-ethoxy-2,3-difluorobromobenzene (T-2) was obtained as a colorless oily matter (230.0 g, yield: 97%).

WORKUP

后处理

  1. additionwas added
  2. temperatureheating agitation
  3. customAfter completion of the reaction, extraction
  4. washan organic layer was washed with water
  5. dry with materiala saturated aqueous solution of sodium chloride, and then the resultant solution was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customthus a black oily matter was obtained
  8. distillationThe resultant material was purified by distillation