반응 #8322

반응 방정식

2-(4-fluoro-phenyl)-3-oxo-3-(6-tri fluoromethyl-pyridin-2-yl)-propionitrile

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title compound

수율 65.5%

2-(4-Fluoro-phenyl)-1-(6-trifluoromethyl-pyridin-2-yl)-ethanone

수율 65.5%

용매

HBr

반응 조건

후처리

1. 1
   온도to reflux for 8 h
2. 2
   온도warmed
3. 3
   온도at reflux for 8 h
4. 4
   추출The mixture is extracted with ether
5. 5
   workup.ADDITIONtreated with a small amount of sodium bicarbonate
6. 6
   추출extracted with ether
7. 7
   추출extracted again with ether
8. 8
   건조dried over magnesium sulfate
9. 9
   농축concentrated in vacuo to a dark oil
10. 10
    기타The residual oil is purified on a silica gel cartridge
11. 11
    기타prepared with hexane
12. 12
    세척then eluted with methylene chloride

실험 절차

A slurry of 2-(4-fluoro-phenyl)-3-oxo-3-(6-tri fluoromethyl-pyridin-2-yl)-propionitrile (1.4 g, 4.4 mmol) in 48% HBr is warmed to reflux for 8 h, allowed to stand at ambient temperature 16 h, then warmed at reflux for 8 h. The mixture is extracted with ether, treated with a small amount of sodium bicarbonate, extracted with ether, made basic with solid sodium hydroxide, and extracted again with ether. Ethereal extracts are combined, dried over magnesium sulfate, and concentrated in vacuo to a dark oil. The residual oil is purified on a silica gel cartridge prepared with hexane then eluted with methylene chloride to yield 816 mg (65%) of the title compound as a dark oil.

출처