反应详情

To a solution of 5-nitro-2-(pyridazin-3-yl)pyrimidin-4-ol, 35i-g, (3.0 g, 13.6 mmol) in THF/H2O (100 mL, VTHF/H2O=1:1) was added Na2S204 (4.77 g, 27.4 mmol) and stirred at room temperature for 4 h. The reaction mixture was extracted with EA (100 mL), washed with brine (50 mL), and concentrated under vacuum. The residue was purified by column chromatography to afford the product, 35i-h, (0.8 g, 30%) as a yellow solid. 1H NMR (300 MHz, CD3OD) δ5.66 (s, 2H), 7.39 (s, 1H), 7.80 (dd, J=4.8, 8.4 Hz, 1H), 8.29 (d, J=8.4 Hz, 1H), 9.26 (d, J=4.8 Hz), LC-MS (M+H)+ 190.1.

1. extractionThe reaction mixture was extracted with EA (100 mL)
2. washwashed with brine (50 mL)
3. concentrationconcentrated under vacuum
4. customThe residue was purified by column chromatography