反应详情

To a solution of 4-[6-(3-Chloro-phenylamino)-pyridazin-3-yl]-benzoic acid (0.10 g, 0.31 mmol, 1.0 equiv) in 2 Ml DMF was added HATU (0.23 g, 0.62 mmol, 2.0 equiv) and N,N-diisopropylethylamine (0.27 Ml, 1.5 mmol, 5.0 equiv). Valine methyl ester (0.062 g, 0.37 mmol, 1.0 equiv) was added as a solid, and the homogeneous solution was allowed to stir at room temperature overnight. To the solution was then added 1 Ml 10% aqueous LiOH, and the mixture was then heated to 55° C. The reactions were then filtered and the purified by reverse-phase HPLC to afford the title compound: 1H NMR (400 MHz, MeOD) δ 0.96 (dd, J=9.35, 6.82 Hz, 6H) 2.21 (dq, J=12.13, 6.82 Hz, 1H) 4.41 (d, J=5.05 Hz, 1H) 6.91 (ddd, J=1.26 Hz, 2.02, 1.01 Hz, 1H) 7-21 (t, J=8.08 Hz, 1H) 7.17 (d, J=9.35 Hz, 1H) 7.48 (dd, J=9.22, 1.14 Hz, 1H) 7.88-8.02 (m, 7H); (M+H)+425.1.

1. temperaturethe mixture was then heated to 55° C
2. filtrationThe reactions were then filtered
3. customthe purified by reverse-phase HPLC