反应详情

温度

130 °C

A mixture of compound 33 (2.03 g, 7.43 mmol), 3-chloropyridin-4-ylboronic acid (3.51 g, 22.3 mmol), and Pd(PPh3)2Cl2 (0.522 g, 0.743 mmol) in dioxane (44 ml) in a pressure vessel was purged with N2 for 20 minutes and to this mixture was added aq. Na2CO3 (1 M, 22 mL) by syringe. The reaction was further purged with N2 for another 20 minutes and then heated to 130° C. for 12 hours. DCM was added to the reaction and the mixture was washed with water and brine. The organic layer was dried with sodium sulfate and concentrated to provide compound 34 (2.07 g, crude, 98%) which was used in the next reaction without further purification. LCMS-ESI (POS), M/Z, M+1: Found 306.1, Calculated 306.1.

1. customwas purged with N2 for 20 minutes and to this mixture
2. additionwas added aq. Na2CO3 (1 M, 22 mL) by syringe
3. customThe reaction was further purged with N2 for another 20 minutes
4. additionDCM was added to the reaction
5. washthe mixture was washed with water and brine
6. dry with materialThe organic layer was dried with sodium sulfate
7. concentrationconcentrated