HRID972835

反应详情

EQUATION

反应方程式

HRID 972835 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 20.6 g of ethyl 2-bromo-4-oxo-butyrate, 10.9 g of thiobutyramide and 400 ml of dichloroethane was refluxed under a nitrogen atmosphere which recycling the dehydrated condensate. The mixture was cooled and then mixed with 45 ml of a saturated sodium bicarbonate aqueous solution. The mixture was decanted and the organic phase was dried and evaporated to dryness. The liquid residue was chromatographed over silica gel and elution with a 8-2 cyclohexane-benzene mixture yielded 15.4 g of ethyl 2-propyl-5-thiazole-acetate. The IR spectrum in CHCl3 showed an ester carbonyl at 1737cm-1 and C=C at 1536cm-1

WORKUP

后处理

  1. temperaturewas refluxed under a nitrogen atmosphere which
  2. temperatureThe mixture was cooled
  3. customThe mixture was decanted
  4. customthe organic phase was dried
  5. customevaporated to dryness
  6. customThe liquid residue was chromatographed over silica gel and elution with a 8-2 cyclohexane-benzene mixture