反应详情

温度

50 °C

4-hydroxy-2-(pyridazin-3-yl)pyrimidine-5-carboxylic acid, 30-ie, (325 mg, 1.5 mmol) and diethyl 4-(amino(4-methoxyphenyl)methyl)benzylphosphonate, 32-f, (540 mg, 1.5 mmol) was dissolved in DMF (5 ml), HATU (570 mg, 1.5 mmol) and DIEA (590 mg, 4.5 mmol) were then added, the reaction mixture was stirred for 2 h at 50° C. under nitrogen. The resulting mixture was cooled to ambient temperature, diluted with water (10 ml), filtered, the residue was washed with water for 3 times, a brown solid was obtained, 32-g, (500 mg, 60% yield). 1H NMR (300 MHz, DMSO-d6) δ 1.14-1.18 (t, J=4.2 Hz 6H), 3.16-3.23 (d, J=21.3 Hz 2H), 3.73 (s, 3H) 3.89-3.98 (m, 4H), 6.20-6.22 (d, J=7.8 Hz, 1H), 6.89-6.92 (m, 2H), 7.20-7.24 (m, 6H), 7.99-8.02 (m, 1H), 8.49-8.58 (m, 2H), 9.48-9.50 (m, 1H), 14.00 (s, 1H). LC-MS 564 [MH]+.

1. temperatureThe resulting mixture was cooled to ambient temperature
2. filtrationfiltered
3. washthe residue was washed with water for 3 times
4. customa brown solid was obtained