反应详情

温度

100 °C

2-Amino-5-[2-fluoro-4-(1-hydroxy-1-methylethyl)phenyl]thiophene-3-carboxamide (100 mg, 0.34 mmol), 4-[(4-chloropyrimidin-2-yl)methyl]morpholine (72.6 mg, 0.34 mmol), Pd2 dba3 (31.1 mg, 0.03 mmol), K2CO3 (51.6 mg, 0.37 mmol) and X-Phos (81 mg, 0.17 mmol) were combined in a 2 mL microwave vial. Degassed tert-amyl alcohol (0.7 mL) was added and the vial evacuated and back-filled with N2 (3×). The resulting mixture was stirred at 100° C. for 24 hours. The reaction mixture was cooled to room temperature, MeOH was added and the reaction mixture was filtered through Celite. The filtrate was combined with silica gel and concentrated in vacuo. Purification of the residue by silica gel chromatography (0-20% MeOH-EtOAc) gave the title compound as a pale yellow solid.

1. customthe vial evacuated
2. additionback-filled with N2 (3×)
3. temperatureThe reaction mixture was cooled to room temperature
4. additionMeOH was added
5. filtrationthe reaction mixture was filtered through Celite
6. concentrationconcentrated in vacuo
7. customPurification of the residue by silica gel chromatography (0-20% MeOH-EtOAc)