HRID975248
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureat reflux for 4 h
- customThe solvent was evaporated in vacuo
- extractionthe residue extracted with dichloromethane (2×100 ml)
- washThe combined organic phases were washed with water (2×50 ml) and brine (10 ml)
- dry with materialdried (MgSO4)
- customThe solvent was evaporated in vacuo
- waitthe residue left for crystallisation
- customthe precipitate collected