HRID1105643

反应详情

EQUATION

反应方程式

HRID 1105643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

0.326 g. of 7-(3-Hydroxy-5-oxo-1-cyclopenten-1-yl)-heptanoic acid were dissolved in 20 ml. of dry acetone. At -20° C., 0.23 ml. of triehtylamine were added and then 0.216 ml. isobutyl chloroformate. After 5 minutes, the temperature was permitted to increase to 25° C., and 0.4 g. of p-benzoylaminophenol dissolved in 10 ml. of dry pyridine was added dropwise. After 2 hours, the solvent was distilled off; the residue was extracted in ethyl acetate; the organic phase was washed with water and dried over sodium sulphate. The solvent was distilled off. After chromatographic purification of the residue (silica gel/ethyl acetate), 7-(3-hydroxy-5-oxo-1-cyclopenten-1-yl)-heptanoic acid p-benzoylaminophenyl ester (m.p. 168°-169° C.) was obtained.

WORKUP

后处理

  1. customAt -20° C.
  2. waitAfter 2 hours
  3. distillationthe solvent was distilled off
  4. extractionthe residue was extracted in ethyl acetate
  5. washthe organic phase was washed with water
  6. dry with materialdried over sodium sulphate
  7. distillationThe solvent was distilled off
  8. customAfter chromatographic purification of the residue (silica gel/ethyl acetate)