HRID1758985

反应详情

EQUATION

反应方程式

HRID 1758985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturethe mixture refluxed for 6 hours
  2. temperatureThe reaction mixture was cooled
  3. extractionthe mixture extracted with ethyl acetate
  4. washThe combined ethyl acetate extracts were washed with water
  5. dry with materialThe ethyl acetate layer was dried (MgSO4)
  6. customevaporated