반응 #2507818

반응 방정식

caesium carbonate

o-phenylphenol

6-fluoro-7-iodo-3-propylchroman

diethyl malonate

→

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

용매

ether

THF

반응 조건

후처리

1. 1
   온도the mixture is heated
2. 2
   온도under reflux overnight
3. 3
   세척is washed with dil. hydrochloric acid
4. 4
   건조dried over sodium sulfate
5. 5
   기타The solvent is removed in vacuo
6. 6
   기타the crude product is purified by chromatography on silica gel with heptane/ethyl acetate (4:1)
7. 7
   기타The product fraction (Rf=0.55) is reacted without further purification

실험 절차

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.

출처