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 suspension of alminium chloride (4.62 g, 34.7 mmol) in ethylene chloride (50 mL) was added under a nitrogen atmosphere p-toluoyl chloride (4.91 g, 31.8 mmol) in ethylene chloride (5 mL) at room temperature in a period of 10 minutes. After stirring for 30 minutes to the mixture was added 1-benzenesulfonyl-1H-pyrrole (6.00 g, 28.9 mmol) in ethylene chloride (10 mL) in a period of 10 minutes. After stirring for 2 hours at room temperature, the reaction mixture was poured into ice water and the aqueous layer was extracted twice with dichloromethane. The organic layer combined was dried over magnesium sulfate and filtered. The filtrate was concentrated and the residue was purified by silica gel column chromatography to give the subject compound (9.9 g, 100%).
WORKUP
后处理
- stirringAfter stirring for 2 hours at room temperature
- extractionthe aqueous layer was extracted twice with dichloromethane
- dry with materialThe organic layer combined was dried over magnesium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated
- customthe residue was purified by silica gel column chromatography