HRID389685

反应详情

EQUATION

反应方程式

HRID 389685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-Bromo-2-fluoro-3-nitro-benzene (3 g, 13.64 mmol), iron (2.28 g, 40.91 mmol), water (34.39 ml, 1909 mmol) and acetic acid (11.7 ml, 204.55 mmol) were added to ethanol (60 ml) and heated to reflux for 2 h. The reaction mixture was then filtered through Celite and evaporated. Water was added and the solution was made basic by the addition of 2 N NaOH, followed by extraction with DCM. The organic layers were washed with water and brine, dried with Na2SO4 evaporated to dryness and the crude product was obtained and used without further purification. Yield: 1.46 g, 56%

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 2 h
  3. filtrationThe reaction mixture was then filtered through Celite
  4. customevaporated
  5. additionWater was added
  6. additionthe solution was made basic by the addition of 2 N NaOH
  7. extractionfollowed by extraction with DCM
  8. washThe organic layers were washed with water and brine
  9. dry with materialdried with Na2SO4
  10. customevaporated to dryness