HRID62634
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
1-Benzyl-3-(3,5-dichlorophenyl)-4-(phenylsulfinyl)-3-(trifluoromethyl)pyrrolidinium chloride (1.00 g, 82% purity, 1.53 mmol) is suspended in toluene (3 mL) under a nitrogen atmosphere. Sodium carbonate (810 mg, 7.65 mmol) was added and the mixture was heated to reflux for 2.5 hours. After cooling water was added, the phases were separated and the aqueous phase was extracted twice with toluene. The combined organic phases were dried over sodium sulphate, filtered and the solvent evaporated. The residue was repeatedly crystallized from n-heptane to yield 1-benzyl-3-(3,5-dichlorophenyl)-3-(trifluoromethyl)-2,3-dihydro-1H-pyrrole (198 mg, 89% purity, 31% yield).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureto reflux for 2.5 hours
- additionwas added
- customthe phases were separated
- extractionthe aqueous phase was extracted twice with toluene
- dry with materialThe combined organic phases were dried over sodium sulphate
- filtrationfiltered
- customthe solvent evaporated
- customThe residue was repeatedly crystallized from n-heptane