反应详情

The 4-hydroxy-2-(pyridin-2-yl)pyrimidine-5-carboxylic acid, 1-1-h, (500 mg, 2.3 mmol) was dissolved in SOCl2 (10 ml), the mixture was stirred at RT for 3 hours, then concentrated under vacuo. The residue was dissolved with 20 ml DCM, and dropwise to a solution of diethyl 3-(amino(4-methoxyphenyl)methyl)phenylphosphonate hydrochloride (5-d, 802 mg, 2.30 mmol) and Et3N (464 mg, 4.6 mmol) in DCM (30 ml) at 0° C., the mixture was stirred at room temperature overnight. Then added water, the water phase was concentrated under vacuo and purified on silica gel chromatography to provide the product, 5-e, (990 mg, 78.4%).

1. concentrationconcentrated under vacuo
2. dissolutionThe residue was dissolved with 20 ml DCM
3. concentrationThen added water, the water phase was concentrated under vacuo
4. custompurified on silica gel chromatography