반응 #626438

반응 방정식

2′-fluoro-2,3-dimethoxybiphenyl-4-boronic acid

2-fluoro-5-bromoiodobenzene

sodium carbonate

→

5-bromo-2-fluoro-2′,3′-dimethoxy-2″-fluoro-p-terphenyl

수율 80.1%

용매

toluene

반응 조건

후처리

1. 1
   온도with heating
2. 2
   온도under reflux for 8 hours
3. 3
   추출the reaction solution was extracted with toluene
4. 4
   기타An aqueous phase was removed
5. 5
   세척an organic phase was washed with saturated saline
6. 6
   건조The organic phase was dried with magnesium sulfate
7. 7
   농축concentrated
8. 8
   기타Residues were purified by means of silica gel column chromatography

실험 절차

In the atmosphere of argon, 15.2 g of 2′-fluoro-2,3-dimethoxybiphenyl-4-boronic acid, 16.5 g of 2-fluoro-5-bromoiodobenzene, 1.27 g of tetrakistriphenylphosphine palladium (0), 180 mL of toluene and 90 mL of an aqueous 2M sodium carbonate solution were placed in a flask. The resulting solution was stirred with heating under reflux for 8 hours. After cooling to room temperature, the reaction solution was extracted with toluene. An aqueous phase was removed, and an organic phase was washed with saturated saline. The organic phase was dried with magnesium sulfate, and concentrated. Residues were purified by means of silica gel column chromatography, whereby 17.8 g (yield: 80%) of 5-bromo-2-fluoro-2′,3′-dimethoxy-2″-fluoro-p-terphenyl was obtained.

출처