反应详情

460 mg of iron are added to a solution of 460 mg of [(2-fluoro-5-nitrophenyl)ethynyl](trimethyl)silane in 10 ml of methanol, and the medium is adjusted to pH 4-5 with concentrated hydrochloric acid. After refluxing for three and a half hours, the medium is cooled and then filtered through silica, and concentrated to dryness under reduced pressure. The residue is taken up with diethyl ether, the insoluble material is filtered off, and then the filtrate is concentrated to dryness under reduced pressure. 370 mg of 4-fluoro-3-[(trimethylsilyl)ethynyl]aniline are obtained in the form of an orangey oil, the characteristics of which are the following:

1. temperatureAfter refluxing for three and a half hours
2. temperaturethe medium is cooled
3. filtrationfiltered through silica
4. concentrationconcentrated to dryness under reduced pressure
5. filtrationthe insoluble material is filtered off
6. concentrationthe filtrate is concentrated to dryness under reduced pressure