HRID1723609

反应详情

EQUATION

反应方程式

HRID 1723609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

The sodium salt of 4-hydroxybutyric acid (1.26 g; 10 mmol) is dissolved in anhydrous pyridine (30 ml), and 4,4′-dimethoxytrityl chloride (3.39 g; 3.05 mmol) is added. After 16 hours, 4-nitrophenol (1.39 g; 10 mmol) and N,N′-dicyclohexylcarbodiimide (2.06 g; 10 mmol) are added, and the mixture is stirred at 22° C. for a further 48 hours. The precipitated dicyclohexylurea is filtered off and washed with dichloromethane. The filtrate is concentrated and the resulting residue is coevaporated twice with toluene. The residue is purified on a silica gel column (10-50% ethyl acetate and 1% triethylamine in petroleum ether). The desired compound is obtained in the form of a pale yellowish-colored oil.

WORKUP

后处理

  1. filtrationThe precipitated dicyclohexylurea is filtered off
  2. washwashed with dichloromethane
  3. concentrationThe filtrate is concentrated
  4. customThe residue is purified on a silica gel column (10-50% ethyl acetate and 1% triethylamine in petroleum ether)