HRID246642
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
- 30 °C
PROCEDURE
实验过程
A mixture of 6-chloro-1H-indazole (2 g, 13.1 mmol), KOH (2.2 g, 39.3 mmol) and I2 (6.6 g, 26.2 mmol) in dry DMF (20 mL) was heated to 30° C. for 16 hours. Reaction quenched with water, product was extracted with ethyl acetate (150 mL), organic phase washed with water (3×10 mL), brine (2×10 mL) and dried over Na2SO4, then filtered and concentrated to afford 6-chloro-3-iodo-1H-indazole (3.0 g, 83%) as a yellow solid. LCMS: (M+H)+=279.
WORKUP
后处理
- customReaction
- customquenched with water, product
- extractionwas extracted with ethyl acetate (150 mL), organic phase
- washwashed with water (3×10 mL), brine (2×10 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated