HRID257418

反应详情

EQUATION

反应方程式

HRID 257418 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Chloro-3-nitropyridine (1.50 g, 9.46 mmol) and aniline (2.0 ml, 21.9 mmol) were dissolved in 10 ml of 1,4-dioxane, and 2 ml of triethylamine was added thereto, followed by reaction at 80° to 90° C. for 2 hours. Then, the solvent was removed by distillation under reduced pressure, and 10 ml of hexane was added to the residue to wash it. The solvent was removed by decantation. The residue was further similarly treated with 10 ml of ether. The residue was purified by silica gel column chromatography [eluent: hexane:ethyl acetate=2:1 (v/v)]to obtain 1.41 g of a yellow solid (yield: 68.8%).

WORKUP

后处理

  1. customfollowed by reaction at 80° to 90° C. for 2 hours
  2. customThen, the solvent was removed by distillation under reduced pressure, and 10 ml of hexane
  3. additionwas added to the residue
  4. washto wash it
  5. customThe solvent was removed by decantation
  6. additionThe residue was further similarly treated with 10 ml of ether
  7. customThe residue was purified by silica gel column chromatography [eluent