HRID62634

反应详情

EQUATION

反应方程式

HRID 62634 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 2.5 hours
  3. additionwas added
  4. customthe phases were separated
  5. extractionthe aqueous phase was extracted twice with toluene
  6. dry with materialThe combined organic phases were dried over sodium sulphate
  7. filtrationfiltered
  8. customthe solvent evaporated
  9. customThe residue was repeatedly crystallized from n-heptane