反应详情

温度

95 °C

A solution of 8-chloro-2-(methylthio)pyrido[3,4-d]pyrimidine (Preparation 33, 20 mg, 0.094 mmol), cyclopropyl boronic acid (11 mg, 0.128 mmol), PCy3 (3 mg, 10.70 μmol), and Pd(OAc)2 (1 mg, 4.45 μmol) was dissolved in toluene/water 6:1 (1 mL) and heated to 95° C. for 18 hours. The mixture was diluted with EtOAc and quenched with brine. The aqueous layer was extracted with EtOAc three times. The combined organic layers were washed with water and brine, dried and concentrated. The residue was purified by silica gel column chromatography eluting with 0 to 20% EtOAc in cyclohexane to give the title compound (13 mg, 62%).

1. customquenched with brine
2. extractionThe aqueous layer was extracted with EtOAc three times
3. washThe combined organic layers were washed with water and brine
4. customdried
5. concentrationconcentrated
6. customThe residue was purified by silica gel column chromatography
7. washeluting with 0 to 20% EtOAc in cyclohexane