HRID388924

反应详情

EQUATION

反应方程式

HRID 388924 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 a solution of 2-fluoro-4-nitrobenzonitrile (10 mmol) in isopropanol (30 mL) was added aqueous hydrazine (4 mL). The resulting solution was heated at 80° C. for 12 h. The reaction mixture was then concentrated, water (30 mL) was added, and the solution was extracted with ethyl acetate (2×25 mL). The combined organics were washed with water (30 mL) and brine (30 mL) and dried over anhydrous sodium sulfate. The volatiles were removed in vacuo yielding 3-amino-6-nitroindazole as an orange solid, which was utilized for further transformation without further purification.

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated
  2. additionwater (30 mL) was added
  3. extractionthe solution was extracted with ethyl acetate (2×25 mL)
  4. washThe combined organics were washed with water (30 mL) and brine (30 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe volatiles were removed in vacuo