HRID1683743

反应详情

EQUATION

反应方程式

HRID 1683743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-phenyl-1-indanone (4.2 g, 20 mmol, J. Chem. Soc. 1949, 2957), hydroxylammonium chloride (2.8 g, 40 mmol) and pyridine (30 ml) was heated at reflux overnight. The reaction mixture was allowed to cool and the solvent was evaporated in vacuo. The residue was dissolved in ethyl acetate and washed with excess 10% citric acid solution. The organic phase was dried (MgSO4) and the solvent evaporated in vacuo to give a solid which was triturated with a mixture of cyclohexane and ethyl acetate. The solid was isolated by filtration and dried in air to give 2.8 g of 3-phenyl-1-indanone oxime as a solid. M.p. 123°-125° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. temperatureto cool
  4. customthe solvent was evaporated in vacuo
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washwashed with excess 10% citric acid solution
  7. dry with materialThe organic phase was dried (MgSO4)
  8. customthe solvent evaporated in vacuo
  9. customto give a solid which
  10. customwas triturated with a mixture of cyclohexane and ethyl acetate
  11. customThe solid was isolated by filtration
  12. customdried in air