HRID415648

反应详情

EQUATION

反应方程式

HRID 415648 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To the solution of 2,5-Dibromo-3-nitro-pyridine (10.30 g, 35.47 mmol) in the 100 ml of ethanol was added SnCl2 (24.0 g, 106.42 mmol) slowly. The reaction mixture was heated at 80° C. for 2 h. After the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure. Water (250 mL) was added, white solid separated out, then, basified the reaction mixture with NaOH Solution. To this added the 250 ml of ethyl acetate. Filtered it and washed the residue with ethyl acetate, layers are separated, dried (Na2SO4), filtered, concentrated to give the desired product (6.20 g, 67.39%).

WORKUP

后处理

  1. customAfter the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure
  2. additionWater (250 mL) was added
  3. customwhite solid separated out
  4. additionTo this added the 250 ml of ethyl acetate
  5. filtrationFiltered it
  6. washwashed the residue with ethyl acetate, layers
  7. customare separated
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated