反应 #2507818

反应方程式

caesium carbonate

o-phenylphenol

6-fluoro-7-iodo-3-propylchroman

diethyl malonate

→

Diethyl 2-(6-fluoro-3-propylchroman-7-yl)malonate

溶剂

ether

THF

反应条件

后处理

1. 1
   温度the mixture is heated
2. 2
   温度under reflux overnight
3. 3
   洗涤is washed with dil. hydrochloric acid
4. 4
   干燥dried over sodium sulfate
5. 5
   其他The solvent is removed in vacuo
6. 6
   其他the crude product is purified by chromatography on silica gel with heptane/ethyl acetate (4:1)
7. 7
   其他The product fraction (Rf=0.55) is reacted without further purification

实验过程

17.0 g (52.2 mmol) of anhydrous caesium carbonate, 700 mg (3.67 mmol) of copper(I) iodide and 700 mg (4.11 mmol) of o-phenylphenol are initially introduced under dry nitrogen, a solution of 11.4 g (33.5 mmol) of 6-fluoro-7-iodo-3-propylchroman and 16.0 g (100 mmol) of diethyl malonate in 150 ml of THF is added, and the mixture is heated under reflux overnight. MTB ether is subsequently added to the batch, which is washed with dil. hydrochloric acid and dried over sodium sulfate. The solvent is removed in vacuo, and the crude product is purified by chromatography on silica gel with heptane/ethyl acetate (4:1). The product fraction (Rf=0.55) is reacted without further purification.

来源