HRID1452050

反应详情

EQUATION

反应方程式

HRID 1452050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 4-ethyl-2-nitro-6-bromoaniline (6.62g, 27mmol) in ethanol (40mL). Add, by dropwise addition, concentrated sulfuric acid (5mL) and heat at reflux, adding sodium nitrite (4.55g, mmol) in small portions over 25 minutes. Stir at room temperature for several hours, pour onto ice and extract into ethyl acetate. Wash with water (3×) and brine (3×). Dry (MgSO4) and evaporate the solvent in vacuo and purify by silica gel chromatography to give 3-bromo-5-ethylnitrobenzene.

WORKUP

后处理

  1. temperatureheat
  2. temperatureat reflux
  3. additionpour onto ice
  4. extractionextract into ethyl acetate
  5. washWash with water (3×) and brine (3×)
  6. dry with materialDry (MgSO4)
  7. customevaporate the solvent in vacuo
  8. custompurify by silica gel chromatography