HRID388934
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe reaction mixture was concentrated
- additionadded with 5% aqueous Na2CO3 solution (20 mL)
- extractionextracted with EtOAc (2×15 mL)
- washThe combined organics were then washed with water (20 mL) and brine (20 mL)
- dry with materialdried over anhydrous Na2SO4
- customRemoval of volatiles