반응 #1933178

반응 방정식

4-bromo-1-fluoro-2-iodobenzene

4-sulfamoyl-phenylboronic acid

dioxane H2O

Na2CO3

→

desired product

수율 55.0%

5′-Bromo-2′-fluorobiphenyl-4-sulfonamide

수율 55.0%

용매

EtOAc

water

반응 조건

후처리

1. 1
   온도cooled
2. 2
   추출The aqueous layer was extracted with EtOAc
3. 3
   건조the combined organic layers dried over Na2SO4
4. 4
   기타The solvent was removed in vacuo
5. 5
   기타the resulting residue purified via silica gel column chromatography
6. 6
   세척eluting with EtOAc:heptanes 0:1 to 1:1

실험 절차

To 4-bromo-1-fluoro-2-iodobenzene (361 mg, 1.2 mmol) and 4-sulfamoyl-phenylboronic acid (240 mg, 1.20 mmol) in 4:1 dioxane/H2O (5 mL) was added Na2CO3 (382 mg, 3.60 mmol) and [1,1′-Bis(diphenylphosphino)-ferrocene]dichloropalladium(II) (34.3 mg, 0.042 mmol). The reaction was heated under microwave irradiation at 120° C. for 15 minutes, cooled and diluted with EtOAc and water. The aqueous layer was extracted with EtOAc and the combined organic layers dried over Na2SO4. The solvent was removed in vacuo and the resulting residue purified via silica gel column chromatography eluting with EtOAc:heptanes 0:1 to 1:1 to afford the desired product 55%, 218 mg, 55%.

출처