反应详情

A mixture of 5-amino-2-(pyridazin-3-yl)pyrimidin-4-ol, 35i-h, (0.5 g, 2.6 mmol), 2-(3-(diethoxyphosphoryl)phenyl)acetic acid, 35i-d, (0.7 g, 2.6 mmol), HATU (1.5 g, 3.9 mmol) and Et3N (1.2 g, 11.8 mmol) in MeCN (25 mL) was stirred at room temperature overnight. The reaction mixture was concentrated in vacuum. The residue was extracted with EA (100 mL), and then washed with sat. NH4Cl (50 mL), water (50 mL), and brine (50 mL). The organic layer was concentrated and the residue was purified by column chromatography to afford the product, 35i, (280 mg, 25%). LC-MS (M+H)+ 444.1.

1. concentrationThe reaction mixture was concentrated in vacuum
2. extractionThe residue was extracted with EA (100 mL)
3. washwashed with sat. NH4Cl (50 mL), water (50 mL), and brine (50 mL)
4. concentrationThe organic layer was concentrated
5. customthe residue was purified by column chromatography