反応 #2507818

反応方程式

caesium carbonate

o-phenylphenol

6-fluoro-7-iodo-3-propylchroman

diethyl malonate

→

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

溶媒

ether

THF

反応条件

後処理

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

実験手順

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.

出典