反应详情

温度

150 °C

A suspension of 4-(9-phenyl[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl)benzaldehyde (4-2, 0.80 g, 2.3 mmol) and 2-amino-2,4-dimethylpentanoic acid (3-7, 0.340 g, 2.3 mmol) in DMF (10 mL) was heated at 150° C. for 30 min. The reaction mixture cooled and the solvent was removed in vacuo. The crude residue was dissolved in 3N HCl (8 mL) and was heated at 100° C. for 30 min. The mixture was cooled and purified via reverse phase HPLC (5-65% acetonitrile/water over 15 min) to give, upon evaporation of the solvents, the title compound as a yellow solid. 1H-NMR (CD3OD) δ 9.60 (s, 1H), 8.98 (s, 1H), 8.73 (d, 1H), 7.75 (d, 1H), 7.60 (d, 2H), 7.46 (d, 2H), 7.39-7.36 (m, 5H), 4.15 (s, 2H).

1. temperatureThe reaction mixture cooled
2. customthe solvent was removed in vacuo
3. dissolutionThe crude residue was dissolved in 3N HCl (8 mL)
4. temperaturewas heated at 100° C. for 30 min
5. temperatureThe mixture was cooled
6. custompurified via reverse phase HPLC (5-65% acetonitrile/water over 15 min)
7. customto give, upon evaporation of the solvents