HRID1706011

反应详情

EQUATION

反应方程式

HRID 1706011 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred ice cold solution of ethyl acetate (75 ml.) containing 3-(acetylthio)propanoic acid (7.4 g. 50 mmol.) and p-nitrophenol (8.4 g., 60 mmol.) dicyclohexylcarbodiimide (10.3 g., 50 mmol.) is added in portions. After thirty minutes, the ice bath is removed and the solution stirred at room temperature overnight. The precipitated dicyclohexylurea is filtered off, ethyl acetate evaporated, and the residue dissolved in ethanol. The 3-(acetylthio)propanoic acid p-nitrophenyl ester crystallizes out, yield 8.6 g. (63.7%), m.p. 71°-73°.

WORKUP

后处理

  1. additionis added in portions
  2. waitAfter thirty minutes
  3. customthe ice bath is removed
  4. filtrationThe precipitated dicyclohexylurea is filtered off
  5. customethyl acetate evaporated
  6. dissolutionthe residue dissolved in ethanol
  7. customThe 3-(acetylthio)propanoic acid p-nitrophenyl ester crystallizes out