HRID544424

反应详情

EQUATION

反应方程式

HRID 544424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

40 g of allyl bromopyruvate were progressively added to a mixture of 30.2 gof phenylthioacetamide, 120 ml of ethanol and 20 ml of pyridine and the mixture was refluxed for 16 hours. The mixture was evaporated to dryness under reduced pressure and the residue was added to a water-ether mixture.The mixture was stirred and the decanted aqueous phase was extracte with ether. The combined organic phases were evaporated to dryness and the residue was chromatographed over silica gel. Elution with a 7-3 hexane-ethyl acetate mixture yielded 22.5 g of ethyl 2-benzyl-thiazole-4-carboxylate melting at 78°-79° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 16 hours
  2. customThe mixture was evaporated to dryness under reduced pressure
  3. additionthe residue was added to a water-ether mixture.The mixture
  4. customThe combined organic phases were evaporated to dryness
  5. customthe residue was chromatographed over silica gel
  6. washElution with a 7-3 hexane-ethyl acetate mixture