反应详情

温度

85 °C

In a 250 mL round-bottomed flask, tert-butyl 6-(6-(6-chloro-2-methyl-3-oxo-2,3-dihydropyridazin-4-ylamino)pyridin-3-yl)-2,6-diazaspiro[3.3]heptane-2-carboxylate (300 mg, 693 μmol), 2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyl acetate (445 mg, 901 μmol) and Cs2CO3 (677 mg, 2.08 mmol) were combined with dioxane (20 ml) and water (2.00 ml) to give a yellow suspension. The flask was evacuated and filled with argon and PdCl2(DPPF) (17.0 mg, 20.8 μmol) was added. The reaction mixture was heated to 85° C. and stirred for 3 h under argon. Additional PdCl2(DPPF) (17 mg, 20.8 μmol) was added and the reaction mixture was heated to 85° C. and stirred for 60 h. Cooled to 25° C. and diluted with DCM. The reaction mixture was filtered through celite and the filtrate was dried over Na2SO4. The crude reaction mixture was concentrated in vacuo. The brown solid was used crude in the subsequent reaction. (M+H)+=765 m/e.

1. customto give a yellow suspension
2. customThe flask was evacuated
3. additionwas added
4. temperaturethe reaction mixture was heated to 85° C.
5. stirringstirred for 60 h
6. temperatureCooled to 25° C.
7. filtrationThe reaction mixture was filtered through celite
8. dry with materialthe filtrate was dried over Na2SO4
9. customThe crude reaction mixture
10. concentrationwas concentrated in vacuo
11. customin the subsequent reaction