HRID1803841

反应详情

EQUATION

反应方程式

HRID 1803841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 85% sodium hydrosulfite (38.1 g, 186 mmol) in water (200 mL) was added dropwise to a mixture of 5-[(3,5-difluorobenzyl)oxy]-2-nitrobenzonitrile (9 g, 31 mmol) and tetrabutylammonium chloride (5.86 g, 21.1 mmol) in dichloromethane (200 mL) under vigorous stirring. After 2 hours, the reaction mixture was cooled at 0° C. and 2N NaOH (200 mL) was added to reach a pH value of 12. The organic phase was separated and the acqueous layer was washed with dichloromethane. Organic phases were collected and treated for 3 hours with 4M hydrochloric acid in dioxane (50 mL). The reaction mixture was washed with water, NaHCO3 saturated solution and brine. Organic phase was dried over sodium sulphate, filtered and evaporated to dryness affording 7.6 g (yield 94%) of the title compound.

WORKUP

后处理

  1. customThe organic phase was separated
  2. washthe acqueous layer was washed with dichloromethane
  3. customOrganic phases were collected
  4. additiontreated for 3 hours with 4M hydrochloric acid in dioxane (50 mL)
  5. washThe reaction mixture was washed with water, NaHCO3 saturated solution and brine
  6. dry with materialOrganic phase was dried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated to dryness