반응 #573545

반응 방정식

3,4-difluorophenylboric acid

2,5-dibromopyridine

ethanol

sodium carbonate

→

5-bromo-2-(3,4-difluorophenyl)pyridine

용매

benzene

반응 조건

후처리

1. 1
   온도is heated
2. 2
   기타(66° C.)
3. 3
   기타for 7 hours
4. 4
   온도After cooling the mixture
5. 5
   추출is extracted with diethyl ether
6. 6
   세척The organic phase is washed with 100 ml of saturated sodium hydrogen carbonate solution and 100 ml of water
7. 7
   건조dried over sodium sulphite
8. 8
   여과filtered
9. 9
   농축concentrated
10. 10
    기타Purification of the residue by chromatography on silica gel with hexane/ethyl acetate 19:1

실험 절차

A mixture of 6.2 g of 3,4-difluorophenylboric acid, 8.5 g of 2,5-dibromopyridine, 0.31 g of tetrakistriphenylphosphine palladium, 60 ml of ethanol, 120 ml of benzene and 120 ml of 2N sodium carbonate solution is heated to boiling (66° C.) for 7 hours while stirring. After cooling the mixture is extracted with diethyl ether. The organic phase is washed with 100 ml of saturated sodium hydrogen carbonate solution and 100 ml of water, dried over sodium sulphite, filtered and concentrated. Purification of the residue by chromatography on silica gel with hexane/ethyl acetate 19:1 yields pure 5-bromo-2-(3,4-difluorophenyl)pyridine.

출처