HRID1683734

反应详情

EQUATION

反应方程式

HRID 1683734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-phenyl-2-cyclohexen-1-one (0.6 g, 3.5 mmol, Tetrahedron 1972, 28, 2369), hydroxylammonium chloride (0.5 g, 7 mmol) and dry pyridine (15 ml) was heated at reflux for 3 h. The reaction mixture was allowed to cool and the solvent was evaporated in vacuo. The residue was dissolved in a mixture of ethyl acetate and water. A 10% citric acid solution was added until acidic pH and the phases were separated. The organic phase was extracted with a 10% citric acid solution and dried (MgSO4). The solvent was evaporated in vacuo to give 0.55 g of 2-phenyl-2-cyclohexen-1 -one oxime. M.p. 144°-146° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 3 h
  3. temperatureto cool
  4. customthe solvent was evaporated in vacuo
  5. dissolutionThe residue was dissolved in a mixture of ethyl acetate and water
  6. additionA 10% citric acid solution was added until acidic pH
  7. customthe phases were separated
  8. extractionThe organic phase was extracted with a 10% citric acid solution
  9. dry with materialdried (MgSO4)
  10. customThe solvent was evaporated in vacuo