HRID1758985
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
Sodium metabisulphite (26 g) in water (60 ml) was added to 1-(4-carbomethoxymethoxyphenyl)propan-2-one oxime (7.5 g) in methanol (50 ml) and the mixture refluxed for 6 hours. The reaction mixture was cooled, concentrated hydrochloric acid (30 ml) added and the mixture extracted with ethyl acetate. The combined ethyl acetate extracts were washed with water followed by sodium bicarbonate solution. The ethyl acetate layer was dried (MgSO4) and evaporated to give the title compound as an oil which crystallised on standing, (mp 63°-70°l ). τ (CDCl3) 7.91 (3H, s), 6.30 (2H, s), 6.26 (3H, s), 5.42 (2H, s), 3.17 (2H, d, J=8 Hz), 2.87 (2H, d, J=8 Hz).
WORKUP
后处理
- temperaturethe mixture refluxed for 6 hours
- temperatureThe reaction mixture was cooled
- extractionthe mixture extracted with ethyl acetate
- washThe combined ethyl acetate extracts were washed with water
- dry with materialThe ethyl acetate layer was dried (MgSO4)
- customevaporated