HRID1281768

反应详情

EQUATION

反应方程式

HRID 1281768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

Ethyl 2-(5-chloro-2-nitroanilino)benzo[b]thiophene-3-carboxylate (3.2 g) was suspended in ethanol (40 ml) and a solution obtained by dissolving tin(II) chloride dihydrate (7.7 g) in ethanol (50 ml) and 18% hydrochloric acid (50 ml) was added with stirring the mixture. The mixture was stirred at 60° C. for 2 hr and cooled to 30° C. Potassium carbonate was added until the reaction mixture was basified. After filtering through celite, the filtrate was extracted with ethyl acetate, washed with water and dried over magnesium sulfate. After natural filtration, the solvent was evaporated under reduced pressure to give ethyl 2-(2-amino-5-chloroanilino)benzo[b]thiophene-3-carboxylate (2.6 g).

WORKUP

后处理

  1. customa solution obtained
  2. additionwas added
  3. stirringThe mixture was stirred at 60° C. for 2 hr
  4. filtrationAfter filtering through celite
  5. extractionthe filtrate was extracted with ethyl acetate
  6. washwashed with water
  7. dry with materialdried over magnesium sulfate
  8. filtrationAfter natural filtration
  9. customthe solvent was evaporated under reduced pressure