反应详情

温度

100 °C

Compound 83 (100 mg, 0.43 mmol), 4-(2-hydroxyethylsulfamoyl)phenylboronic acid (212 mg, 0.87 mmol), Pd(OAc)2 (5 mg, 0.02 mmol), S-Phos (18 mg, 0.04 mmol), and K2CO3 (299 mg, 2.17 mmol) were dissolved in dioxane/H2O (2.2 mL, 10/1, v/v), and stirred overnight at 100° C. The reaction mixture was diluted with H2O/EtOAc, and filtered through an Extrelut column. The column was washed with EtOAc, and the filtrate was concentrated. The crude product was purified via Biotage eluting with a gradient of 0 to 10% MeOH in CH2Cl2. The resulting material was triturated with MeOH, filtered, and dried under vacuum to provide 174 (6 mg, 4% yield) as a light-yellow solid. LC-MS (M+H=396, obsd.=396).

1. filtrationfiltered through an Extrelut column
2. washThe column was washed with EtOAc
3. concentrationthe filtrate was concentrated
4. customThe crude product was purified via Biotage
5. washeluting with a gradient of 0 to 10% MeOH in CH2Cl2
6. customThe resulting material was triturated with MeOH
7. filtrationfiltered
8. customdried under vacuum