反应详情

温度

100 °C

2-Amino-5-[4-(3-fluorooxetan-3-yl)phenyl]thiophene-3-carboxamide (88 mg, 0.301 mmol), 1-[(6-bromopyridin-2-yl)methoxy]-2-methylpropan-2-ol (Example 217 Step 1) (78 mg, 0.301 mmol), Pd2dba3 (27.6 mg, 0.030 mmol), K2CO3 (45.8 mg, 0.331 mmol) and X-Phos (71.8 mg, 0.151 mmol) were added to a 5 mL microwave vial. Degassed tert-amyl alcohol (0.6 mL) was added and the vial evacuated and back-filled with N2 (3×). The resulting mixture was stirred at 100° C. overnight. After cooling to room temperature, the mixture was diluted with methanol, silica gel was added, and the solvent was removed in vacuo. Purification of the residue by flash chromatography (silica, 0-10% MeOH-DCM) followed by flash chromatography (silica, 12-100% EtOAc-hexanes) gave the title compound as a pale yellow solid.

1. customthe vial evacuated
2. additionback-filled with N2 (3×)
3. temperatureAfter cooling to room temperature
4. additionthe mixture was diluted with methanol, silica gel
5. additionwas added
6. customthe solvent was removed in vacuo
7. customPurification of the residue by flash chromatography (silica, 0-10% MeOH-DCM)