反应详情

温度

135 °C

2-Hydroxy-1-(6-chloropyridin-3-yl)-1,9-dihydro-6H-purin-6-one from the above reaction is suspended in a large excess of phosphorous oxychloride (150 mL) and heated to 135° C. for 24 h. The reaction mixture is cooled, evaporated in vacuo, and additional toluene is added and evaporated (2×) under reduced pressure. The resulting sticky brown oil is dissolved in DCM (200 mL), and then neutralized with saturated NaHCO3 (aqueous). The aqueous layer is extracted with DCM (2×200 mL) and dried (MgSO4). The dried extract is filtered and concentrated under vacuum to afford crude product as a light brown solid. The crude product is purified by flash column chromatography using 1-2.5% MeOH/CH2Cl2 to afford the title compound as white solid. 1H NMR (300 MHz, CDCl3) δ 8.33 (s, 1H), 7.78 (s, 1H), 7.58 (d, J=6 Hz, 1H), 7.53 (d, J=6 Hz, 1H).

1. temperatureThe reaction mixture is cooled
2. customevaporated in vacuo, and additional toluene
3. additionis added
4. customevaporated (2×) under reduced pressure
5. dissolutionThe resulting sticky brown oil is dissolved in DCM (200 mL)
6. extractionThe aqueous layer is extracted with DCM (2×200 mL)
7. dry with materialdried (MgSO4)
8. extractionThe dried extract
9. filtrationis filtered
10. concentrationconcentrated under vacuum
11. customto afford crude product as a light brown solid
12. customThe crude product is purified by flash column chromatography