HRID262373

反应详情

EQUATION

反应方程式

HRID 262373 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dicyclohexylcarbodiimide (1.03 g.) is added to a solution of 3-acetylthio-2-carbamoylmethylpropanoic acid (1.02 g.) in pyridine (18 ml.). After five hours stirring at room temperature, the precipitate is filtered off and the filtrate is concentrated to dryness, the residue is dissolved in ethyl acetate and extracted with saturated aqueous bicarbonate. The aqueous phase is acidified and extracted with ethyl acetate. This organic layer is dried and concentrated to dryness. The residue, 3-acetylthio-2-cyanomethylpropanoic acid is crystallized from ether-hexane, m.p. 110°-112°.

WORKUP

后处理

  1. filtrationthe precipitate is filtered off
  2. concentrationthe filtrate is concentrated to dryness
  3. dissolutionthe residue is dissolved in ethyl acetate
  4. extractionextracted with saturated aqueous bicarbonate
  5. extractionextracted with ethyl acetate
  6. customThis organic layer is dried
  7. concentrationconcentrated to dryness
  8. customThe residue, 3-acetylthio-2-cyanomethylpropanoic acid is crystallized from ether-hexane, m.p. 110°-112°