反应详情

温度

100 °C

2-amino-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]thiophene-3-carboxamide (0.1 g, 0.320 mmol), 4-bromophenyl methyl sulfone (0.075 g, 0.320 mmol), Pd2 dba3 (0.029 g, 0.032 mmol), K2CO3 (0.049 g, 0.352 mmol) and X-Phos (0.076 g, 0.160 mmol) were added to a 5 mL microwave vial. Degassed EtOH (1 mL) was added and the vial evacuated and back-filled with N2 (×3). The resulting mixture was stirred at 100° C. overnight. Room temperature was attained, MeOH was added and the solvent removed in vacuo while loading onto silica. Purification of the residue by MPLC (0-10% MeOH—CHCl3) gave 5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-{[4-(methylsulfonyl)phenyl]amino}thiophene-3-carboxamide as a beige solid after triturating in DCM.

1. customthe vial evacuated
2. additionback-filled with N2 (×3)
3. customRoom temperature
4. additionMeOH was added
5. customthe solvent removed in vacuo
6. customPurification of the residue by MPLC (0-10% MeOH—CHCl3)