HRID325812

反应详情

EQUATION

反应方程式

HRID 325812 的结构方程式

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

A mixture of diethyl 2-(5-phthalimidopentyl)-2-propylmalonate (6 g) and 26% hydrochloric acid (36 ml) was heated in a sealed tube at 190° C. for 4 hours. After cooling, insoluble substance was remeved by filtration. The filtrate was concentrated to dryness under reduced pressure and the residue was chromatographed on silica gel column. A fraction eluted with the upper phase of a mixture of butanol:acetic acid:water (4:1:5 volume by volume) was concentrated by dryness to give colorless sticky oil of the desired compound (yield 1.3 g).

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationinsoluble substance was remeved by filtration
  3. concentrationThe filtrate was concentrated to dryness under reduced pressure
  4. customthe residue was chromatographed on silica gel column
  5. washA fraction eluted with the upper phase of a mixture of butanol:acetic acid:water (4:1:5 volume by volume)
  6. concentrationwas concentrated by dryness