HRID22727
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
PROCEDURE
实验过程
To a solution of 2-mercaptoindole (6.7 mmol, 1.0 g) in acetone (20 mL) was added 2-chloro-6-methoxy-pyridazine (144 mmol, 1.52 g) and potassium carbonate (70 mmol, 0.98 g) and the reaction mixture was refluxed for 2 hours. Excess acetone was removed and the residue was partitioned between CHCl3 (20 mL) and H2O (20 mL). The CHCl3 layer was collected, dried, filtered and the filtrate was evaporated to a residue, which was purified by silica gel chromatography (eluent:hexanes:EtOAc::4:1) to obtain 3-methoxy-6-(indole-2-sulfenyl)-pyridazine (31%, 534 mg).
WORKUP
后处理
- temperaturethe reaction mixture was refluxed for 2 hours
- customExcess acetone was removed
- customthe residue was partitioned between CHCl3 (20 mL) and H2O (20 mL)
- customThe CHCl3 layer was collected
- customdried
- filtrationfiltered
- customthe filtrate was evaporated to a residue, which
- customwas purified by silica gel chromatography (eluent:hexanes:EtOAc::4:1)