HRID325812
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureAfter cooling
- filtrationinsoluble substance was remeved by filtration
- concentrationThe filtrate was concentrated to dryness under reduced pressure
- customthe residue was chromatographed on silica gel column
- washA fraction eluted with the upper phase of a mixture of butanol:acetic acid:water (4:1:5 volume by volume)
- concentrationwas concentrated by dryness