反应详情

温度

120 °C

To a solution of 3,5-dibromopyrazin-2-amine (826 mg, 3.27 mmol), (S)—N-(2-hydroxy-1-phenylethyl)-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzamide (600 mg, 1.634 mmol), and PdCl2(dppf).CH2Cl2 adduct (133 mg, 0.163 mmol) in DME (12.3 mL) was added 2 M Na2CO3 (4.08 mL). The reaction mixture was heated at microwave synthesizer (120° C., 10 min). The reaction mixture was worked uup with EtOAc. The organic layer was washed with sat NaHCO3, water and brine, dried over Na2SO4, filtered off, concentrated in vacuo. The crude product was purified with silica flash chromatography eluting with 0-100% of EtOAc (containing 10% of MeOH) in heptane, and triturated with ether to provide 800 mg of (S)-4-(3-amino-6-bromopyrazin-2-yl)-N-(2-hydroxy-1-phenylethyl)benzamide. LCMS (m/z): 415 (MH+), 0.73 min.

1. washThe organic layer was washed with sat NaHCO3, water and brine
2. dry with materialdried over Na2SO4
3. filtrationfiltered off
4. concentrationconcentrated in vacuo
5. customThe crude product was purified with silica flash chromatography
6. washeluting with 0-100% of EtOAc (containing 10% of MeOH) in heptane
7. customtriturated with ether