反应详情

温度

60 °C

4-hydroxy-2-(pyridazin-3-yl)pyrimidine-5-carboxylic acid, 30-ie, (200 mg, 0.92 mmol) was dissolved in SOCl2 (5 ml). The mixture was stirred at 60° C. for 4 hours, then concentrated under vacuo. The residue was dissolved with 5 ml of DCM, and added dropwise to a solution of diethyl 4-(5-(2-aminopropan-2-yl)pyridin-2-yl)phenylphosphonate, 33-g, (353 mg, 0.92 mmol) and Et3N (371 mg, 3.7 mmol) in DCM (10 ml) at 0° C. The mixture was stirred at room temperature for 5 hours and then washed with brine, dried, and concentrated under vacuo to give diethyl 4-(5-(2-(4-hydroxy-2-(pyridazin-3-yl)pyrimidine-5-carboxamido) propan-2-yl)pyridin-2-yl)phenylphosphonate (220 mg, 44%).

1. concentrationconcentrated under vacuo
2. dissolutionThe residue was dissolved with 5 ml of DCM
3. stirringThe mixture was stirred at room temperature for 5 hours
4. washwashed with brine
5. customdried
6. concentrationconcentrated under vacuo