Potassium Carbonate → tert-butyl 6-(4-(N-methylsulfamoyl)phenyl)pyridin-2-ylcarbamate

温度

80 °C

To a solution of 4-(N-methylsulfamoyl)phenylboronic acid (17.2 g, 0.08 mol) and (6-bromo-pyridin-2-yl)carbamic acid tert-butyl ester (21.9 g, 0.08 mol) in DMF (125 mL) and H2O (125 mL) were added Pd(PPh3)4 (9.2 g, 0.008 mol) and K2CO3 (16.6 g, 0.12 mol). The resulting mixture was degassed by gently bubbling argon through the solution for 5 minutes at 20° C. The reaction mixture was then heated at 80° C. for 16 h. The mixture was evaporated under reduced pressure, then poured into H2O, and extracted with EtOAc. The organic phase was dried over Na2SO4, and was evaporated under reduced pressure to give tert-butyl 6-(4-(N-methylsulfamoyl)phenyl)pyridin-2-ylcarbamate (21 g, 58%), which was used in the next step without further purification.

1. customThe resulting mixture was degassed by gently bubbling argon through the solution for 5 minutes at 20° C
2. customThe mixture was evaporated under reduced pressure
3. additionpoured into H2O
4. extractionextracted with EtOAc
5. dry with materialThe organic phase was dried over Na2SO4
6. customwas evaporated under reduced pressure

ORDレコード

ord-ce353bf459394d0491bb9dfe0f139411

出典データセット

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08993600B2