HRID580628

反应详情

EQUATION

反应方程式

HRID 580628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium metabisulphate (131 g) in water (300 ml) was added to 1-(4-carbomethoxyphenyl)propan-2-one oxime (37.5 g) in methanol (200 ml) and the mixture refluxed for 6 hours. The reaction mixture was cooled, concentrated hydrochloric acid (100 ml) added, the mixture extracted with chloroform and the combined chloroform extracts washed with water followed by sodium bicarbonate solution. The chloroform layer was dried (MgSO4) and evaporated to give the title compound as an oil (bp 126°-129°/0.7 mm) which crystallised on standing, (mp 40°-47°). τ (CDCl3) 7.88 (3H, s), 6.28 (2H, s), 6.14 (3H, s), 2.77 (2H, d, J=8 Hz), 2,04 (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 chloroform
  4. washthe combined chloroform extracts washed with water
  5. dry with materialThe chloroform layer was dried (MgSO4)
  6. customevaporated