反应详情

温度

120 °C

In a 5 ml microwave vial were added 1-[(4-bromo-2-pyridinyl)carbonyl]-4-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine (Description 17) (150 mg, 0.314 mmol), 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (Description 5) (129 mg, 0.627 mmol), bis(triphenylphosphine)palladium(II) chloride (44.0 mg, 0.063 mmol), sodium carbonate (100 mg, 0.941 mmol), 1,2-dimethoxyethane (1.5 ml), ethanol (1.0 ml) and water (0.50 ml). The reaction mixture was heated for 20 minutes at 120° C. in the microwave. The crude material was diluted in EtOH and filtered through celite. The filtrate was concentrated in vacuo then diluted with MeOH and filtered through an SCX cartridge (1 g). All material came out with MeOH wash so product concentrated, diluted with MeOH and filtered through a 5 g SCX column (washed with MeOH, eluted with NH3 0.5M in MeOH). The eluted product was concentrated in vacuo then dissolved in MeCN/DMSO 1:1 and purified by MDAP. The desired fractions were combined and concentrated under vacuo to give the title compound (2 mg).

1. filtrationfiltered through celite
2. concentrationThe filtrate was concentrated in vacuo
3. additionthen diluted with MeOH
4. filtrationfiltered through an SCX cartridge (1 g)
5. washwash so product
6. concentrationconcentrated
7. additiondiluted with MeOH
8. filtrationfiltered through a 5 g SCX column (washed with MeOH, eluted with NH3 0.5M in MeOH)
9. concentrationThe eluted product was concentrated in vacuo
10. dissolutionthen dissolved in MeCN/DMSO 1:1
11. custompurified by MDAP
12. concentrationconcentrated under vacuo