반응 #534957

반응 방정식

5-bromo-1,3-difluoro-2-nitrobenzene

cyclopropylboronic acid

K3PO4

NaBr

→

brown crude product

수율 141.0%

5-Cyclopropyl-1,3-difluoro-2-nitrobenzene

수율 141.0%

용매

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONThe mixture was then poured onto water (10 ml)
2. 2
   추출extracted with ethyl acetate (3×20 ml)
3. 3
   건조The combined organics were dried over MgSO4
4. 4
   여과filtered
5. 5
   기타the solvent was evaporated

실험 절차

5-bromo-1,3-difluoro-2-nitrobenzene (D24, 560 mg, 2.35 mmol), cyclopropylboronic acid (1 eq., 2.35 mmol, 0.2 g), K3PO4 (3 eq., 7.1 mmol, 1.50 g), NaBr (1 eq., 2.35 mmol, 0.24 g) and Pd(PPh3)4 (280 mg) were added to 3 ml of dry toluene and the mixture was heated by microwave at 160° C. for 40 minutes. The mixture was then poured onto water (10 ml) and extracted with ethyl acetate (3×20 ml). The combined organics were dried over MgSO4, filtered and the solvent was evaporated to afford 660 mg of brown crude product which was purified by silica gel chromatography (5-20% diethyl ether-40-60° petroleum ether) to afford the title compound as a yellow oil, 300 mg, 64%.

출처