反应详情

A degassed solution of 3-(2-amino-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-yl)-4-methylpyridin-2(1H)-one (250 mg, 0.97 mmol), tert-butyl(4-iodophenyl)carbamate (200 mg, 0.97 mmol), N1,N2-dimethylethane-1,2-diamine (50 mg, 0.49 mmol), copper iodide (40 mg, 0.20 mmol), and potassium phosphate (410 mg, 1.94 mmol) in 2 mL of N-methylpyrrolidone was heated to 70° C. and stirred overnight (17 h). The reaction was complete and allowed to cool to room temperature. The reaction was extracted with EtOAc (3ט5 mL) and with NaHCO3 (2ט10 mL). The crude organic layers were combined, dried over anhydrous Na2SO4 (s), filtered and the concentrated in vacuo. The crude mixture was then purified using the ISCO flash chromatography system using an 0-100% EtOAc/100-0% Hexane gradient mixture. Following concentration of the appropriate fractions the desired product was collected as an off white solid (115 mg, 27%). 1H NMR (DMSO) δ: 9.52 (s, 1H), 7.92 (s, 1H), 7.45-7.52 (m, 2H), 7.41 (d, J=6.7 Hz, 1H), 7.24-7.31 (m, 2H), 6.28 (s, 2H), 6.17 (d, J=7.0 Hz, 1H), 3.96 (br. S, H), 3.29 (s, 2H), 2.66(t, j=5.3 Hz, 2H), 2.18 (s, 3H), 1.39 (s, 9H)

1. extractionThe reaction was extracted with EtOAc (3ט5 mL) and with NaHCO3 (2ט10 mL)
2. dry with materialdried over anhydrous Na2SO4 (s)
3. filtrationfiltered
4. concentrationthe concentrated in vacuo
5. customThe crude mixture was then purified
6. customwas collected as an off white solid (115 mg, 27%)