HRID388934

反应详情

EQUATION

反应方程式

HRID 388934 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 6-nitroindazole (2 mmol) in DCE (5 mL), sulfuryl chloride (10 mmol) was added and the resulting mixture was heated 80° C. for 3-5 h. The reaction mixture was concentrated, added with 5% aqueous Na2CO3 solution (20 mL) and extracted with EtOAc (2×15 mL). The combined organics were then washed with water (20 mL) and brine (20 mL) and dried over anhydrous Na2SO4. Removal of volatiles afforded 3-chloro-6-nitro-1H-indazole as a yellow solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionadded with 5% aqueous Na2CO3 solution (20 mL)
  3. extractionextracted with EtOAc (2×15 mL)
  4. washThe combined organics were then washed with water (20 mL) and brine (20 mL)
  5. dry with materialdried over anhydrous Na2SO4
  6. customRemoval of volatiles