反应详情

温度

83 °C

A suspension of 2,6-dichloropurine (22.0 g, 116.4 mmol), dihydropyran (11.5 mL, 126 mmol) and D-(+)-10-camphorsulfonic acid (2.20 g, 9.47 mmol) in 1,2-dichloroethane (300 mL) was stirred at 83° C. for 16 hours. The initially white suspension, after 2 hrs, turned yellow and then black. The reaction mixture was diluted with CCl3H and then washed with brine. The organic layer is dried over MgSO4, filtered, concentrated and triturated with hexane 3 times to give the desired product. 1HNMR (300 MHz, CCl3D): δ 8.33 (s, 1H), 5.75 (dd, J=10.4 Hz, 2.5 Hz, 1H), 4.18 (m, 2H), 3.79 (m, 2H), 1.84 (m, 4H).

1. waitThe initially white suspension, after 2 hrs
2. washwashed with brine
3. dry with materialThe organic layer is dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customtriturated with hexane 3 times