反应详情

9-(4-Chlorophenyl)-8-(2-chlorophenyl)-9H-purin-6-ol I-(4A-7)b (2.49 g, 6.97 mmol) was suspended in 50 ml of toluene. Triethylamine (1.07 ml, 7.68 mmol) was added followed by addition of POCl3 (720 μl, 7.72 mmol) at room temperature. The reaction was warmed to reflux and stirred for 23 hours to give a clear orange solution. After cooling the reaction to room temperature it was concentrated under reduced pressure, diluted with isopropanol (50 ml) and then concentrated further under reduced pressure until copious amount of precipitate came out of solution. The concentrated suspension was cooled in an ice bath and stirred for 2 hours. The precipitate was collected on a sintered glass funnel and rinsed with cold isopropanol to afford, after drying in vacuo, I-(4A-7)c as an off-white solid (2.13 g, 82%): +ESI MS (M+1) 375.1; 1H NMR (400 MHz, DMSO-d6) δ 8.84 (s, 1H), 7.76 (dd, J=7.46, 1.2 Hz, 1H), 7.58–7.40 (m, 7H).

1. temperatureThe reaction was warmed
2. temperatureto reflux
3. customto give a clear orange solution
4. temperatureAfter cooling
5. customthe reaction to room temperature it
6. concentrationwas concentrated under reduced pressure
7. additiondiluted with isopropanol (50 ml)
8. concentrationconcentrated further under reduced pressure until copious amount of precipitate
9. temperatureThe concentrated suspension was cooled in an ice bath
10. stirringstirred for 2 hours
11. customThe precipitate was collected on a sintered glass funnel
12. washrinsed with cold isopropanol
13. customto afford
14. dry with materialafter drying in vacuo, I-(4A-7)c as an off-white solid (2.13 g, 82%)