HRID975260
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureat reflux for 1 h
- customThe solvent was evaporated in vacuo
- extractionthe resulting mixture was extracted with dichloromethane (2×100 ml)
- washThe combined organic phases were washed with water (50 ml) and brine (10 ml)
- dry with materialdried (MgSO4)
- customThe solvent was evaporated in vacuo