反应详情

温度

160 °C

A suspension of 2-chloro-7-(1-methyl-1H-pyrazol-4-yl)pyrido[2,3-d]pyrimidine (Preparation 55, 7.5 mg, 0.03 mmol), 4-(1,2-dimethyl-1H-imidazol-5-yl)-2-methoxyaniline (Preparation 74, 10 mg, 0.05 mmol), R-(+)BINAP (2 mg, 3 umol), Pd(OAc)2 (0.69 mg, 3 umol), K2CO3 (42 mg, 0.31 mmol) in DMF (3 mL) was stirred at 160° C. under microwave irradiation for 2 hours. The reaction mixture was filtered, diluted with NaCl solution and extracted with EtOAc. The organic layer was purified by SCX-2 column eluting with 2M NH3 in MeOH and concentrated in vacuo. The residue was purified by Biotage silica gel column chromatography eluting with 0-10% MeOH in EtOAc followed by preparative HPLC to afford the title compound (4 mg, 31%).

1. filtrationThe reaction mixture was filtered
2. additiondiluted with NaCl solution
3. extractionextracted with EtOAc
4. customThe organic layer was purified by SCX-2 column
5. washeluting with 2M NH3 in MeOH
6. concentrationconcentrated in vacuo
7. customThe residue was purified by Biotage silica gel column chromatography
8. washeluting with 0-10% MeOH in EtOAc