HRID975248

反应详情

EQUATION

反应方程式

HRID 975248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,2-diphenylethanone (19.6 g, 100 mmol) and hydroxyl ammonium chloride (13.9 g, 200 mmol) in absolute ethanol (200 ml) was heated at reflux for 4 h. The solvent was evaporated in vacuo and the residue extracted with dichloromethane (2×100 ml). The combined organic phases were washed with water (2×50 ml) and brine (10 ml) and dried (MgSO4). The solvent was evaporated in vacuo and the residue left for crystallisation. The crystallised product was suspended in n-heptane/diethylether 20/1 and the precipitate collected to give 5.1 g of 1,2-diphenylethanone oxime.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 4 h
  3. customThe solvent was evaporated in vacuo
  4. extractionthe residue extracted with dichloromethane (2×100 ml)
  5. washThe combined organic phases were washed with water (2×50 ml) and brine (10 ml)
  6. dry with materialdried (MgSO4)
  7. customThe solvent was evaporated in vacuo
  8. waitthe residue left for crystallisation
  9. customthe precipitate collected