HRID975260

反应详情

EQUATION

反应方程式

HRID 975260 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the above ketone (20.6 g, 127 mmol), hydroxylammonium chloride (17.7 g, 254 mmol) and absolute ethanol (200 ml) was heated at reflux for 1 h and then stirred at ambient temperature for 16 h. The solvent was evaporated in vacuo. The residue was suspended in water (200 ml) and the resulting mixture was extracted with dichloromethane (2×100 ml). The combined organic phases were washed with water (50 ml) and brine (10 ml) and dried (MgSO4). The solvent was evaporated in vacuo to give 20.6 g of 3-methylbutyrophenone oxime.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 1 h
  3. customThe solvent was evaporated in vacuo
  4. extractionthe resulting mixture was extracted with dichloromethane (2×100 ml)
  5. washThe combined organic phases were washed with water (50 ml) and brine (10 ml)
  6. dry with materialdried (MgSO4)
  7. customThe solvent was evaporated in vacuo