反应详情

温度

120 °C

In a 5 ml microwave vial were added 2-bromopyridine (0.093 ml, 0.949 mmol), methyl 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-pyridinecarboxylate (300 mg, 1.139 mmol), bis(triphenylphosphine)palladium(II) chloride (133 mg, 0.190 mmol), sodium carbonate (302 mg, 2.85 mmol), 1,2-dimethoxyethane (1.5 ml), ethanol (1.000 ml) and water (0.500 ml). The reaction mixture was heated for 0.5 hours at 120° C. in the microwave. The mixture was diluted with MeOH and filtered through Celite®. The product was concentrated in vacuo then filtered through a 20 g SCX cartridge (washed with MeOH, eluted with 1M NH3 in MeOH) and evaporated in vacuo. The product was triturated with ether and concentrated under vacuo. The product was diluted in DCM then 1 ml of 1M HCl in ether added and the product was concentrated in vacuo then was dissolved in MeCN/DMSO 1:1 and purified by MDAP. The desired fractions were collected and concentrated under vacuo to give the title compound (44 mg).

1. filtrationfiltered through Celite®
2. concentrationThe product was concentrated in vacuo
3. filtrationthen filtered through a 20 g SCX cartridge (washed with MeOH, eluted with 1M NH3 in MeOH)
4. customevaporated in vacuo
5. customThe product was triturated with ether
6. concentrationconcentrated under vacuo
7. additionThe product was diluted in DCM
8. addition1 ml of 1M HCl in ether added
9. concentrationthe product was concentrated in vacuo
10. dissolutionthen was dissolved in MeCN/DMSO 1:1
11. custompurified by MDAP
12. customThe desired fractions were collected
13. concentrationconcentrated under vacuo