반응 #76156

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Ethyl 2,6-dichloro-5-fluoronicotinate

→

2,6-dichloro-5-fluoro nicotinic acid

수율 62.3%

2,6-Dichloro-5-fluoronicotinic acid

수율 62.3%

용매

trifluoro acetic acid

HCl

반응 조건

후처리

1. 1
   온도The mixture was refluxed
2. 2
   온도It was cooled
3. 3
   기타the trifluoroacetic acid was removed under reduced pressure
4. 4
   workup.ADDITIONThe solution was mixed with 150 mL water
5. 5
   여과the resulting precipitate was filtered
6. 6
   세척washed with hexane
7. 7
   기타dried

실험 절차

Ethyl 2,6-dichloro-5-fluoronicotinate (1) (30.0 g) was dissolved in a mixture of 60 mL of trifluoro acetic acid and 60 mL of 7.5 N HCl. The mixture was refluxed with stirring for 26 h. It was cooled and the trifluoroacetic acid was removed under reduced pressure. The solution was mixed with 150 mL water, the resulting precipitate was filtered, washed with hexane and dried to yield 16.5 g of 2,6-dichloro-5-fluoro nicotinic acid (2). m.p.=152-156° C.

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