反应详情

温度

120 °C

A mixture of 4-(7-bromo-3-methyl-3,4-dihydroisoquinolin-2(1H)-yl)-6-(4-methylpiperazin-1-yl)pyrimidin-2-amine (0.313 g, 0.750 mmol, Example 49, Step 6), tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3,6-dihydropyridine-1(2H)-carboxylate (0.301 g, 0.975 mmol, Boron Molecular, Cat. No. BM550), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex with dichloromethane (1:1) (38 mg, 0.045 mmol), potassium carbonate (415 mg, 3.00 mmol) in water (2.2 mL, 120 mmol) and 1,4-dioxane (4.5 mL) was degassed and recharged with nitrogen three times, and then heated at 120° C.) (oil bath temperature) for 2 h. After cooling, the mixture was diluted with ethyl acetate, washed with water and brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column with ethyl acetate in haxene (0-50%) to give the desired product (380 mg, 97.5%). LCMS (M+H)+: m/z=520.3.

1. temperatureAfter cooling
2. washwashed with water and brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by flash chromatography on a silica gel column with ethyl acetate in haxene (0-50%)