HRID1414267

反应详情

EQUATION

反应方程式

HRID 1414267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4'-(1-Oxo-2-phenylbutyl)methanesulfonanilide (31.7 g., 0.100 mole), potassium carbonate (13.8 g., 0.100 mole), and 2-chlorotriethylamine (13.6 g., 0.100 mole) are mixed together in 1 liter of acetonitrile and refluxed 18 hr. The reaction mixture is clarified by filtration and concentrated under reduced pressure. The residual oil is dissolved in ethyl ether and the product extracted therefrom with 1.5N HCl. The aqueous acid extract is washed with ethyl ether and then basified with 50% NaOH. The organic material which separates is extracted into ethyl ether and the extracts are washed with water and brine, and the solution dried (MgSO4). The ether is evaporated and the solid residue is crystallized from hexane to yield 24.1 g. (58% yield), m.p. 76°-77°C.

WORKUP

后处理

  1. temperaturerefluxed 18 hr
  2. filtrationThe reaction mixture is clarified by filtration
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residual oil is dissolved in ethyl ether
  5. extractionthe product extracted
  6. extractionThe aqueous acid extract
  7. washis washed with ethyl ether
  8. extractionThe organic material which separates is extracted into ethyl ether
  9. washthe extracts are washed with water and brine
  10. dry with materialthe solution dried (MgSO4)
  11. customThe ether is evaporated
  12. customthe solid residue is crystallized from hexane
  13. customto yield 24.1 g