反应详情

温度

75 °C

A solution of tert-butyl 4-[(6-bromo-2-{[1-({[tert-butyl(dimethyl)silyl]oxy}methyl)cyclobutyl]methyl}-1-oxo-1,2-dihydroisoquinolin-4-yl)methyl]piperazine-1-carboxylate (Example 27c, 0.153 g) in DMF (4 mL) was treated with N-cyclopropyl-3-fluoro-4-methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (0.077 g), Pd-118 (4.71 mg) and potassium carbonate (0.067 g) under nitrogen. The resulting mixture was stirred at 75° C. for 8 h. The reaction was partitioned between ethyl acetate and water. The aqueous was extracted with ethyl acetate (2×100 mL) before washing the organics with water (3×100 mL) and brine (3×100 mL). The organic was dried (MgSO4), filtered, and evaporated under reduced pressure to afford the crude product. The crude product was purified (SiO2 chromatography, elution with 30% ethyl acetate/isohexane) to afford the subtitle compound (0.099 g) as an oil.

1. customThe reaction was partitioned between ethyl acetate and water
2. extractionThe aqueous was extracted with ethyl acetate (2×100 mL)
3. washbefore washing the organics with water (3×100 mL) and brine (3×100 mL)
4. dry with materialThe organic was dried (MgSO4)
5. filtrationfiltered
6. customevaporated under reduced pressure
7. customto afford the crude product
8. customThe crude product was purified
9. wash(SiO2 chromatography, elution with 30% ethyl acetate/isohexane)