反应详情

温度

80 °C

In 120 ml DMF, 29.3 g of DBU, 32.45 g (0.191 mol) of 2-amino-6-chloropurine were added, stirred at 80° C. for 30 min, then 50 g (0.193 mol) of 2-(diisopropyloxy-phosphonomethoxy)-ethyl chloride was added, the reaction was performed at 100° C. for 8 h, cooled, distilled at a reduced pressure to remove DMF, added with water and ethyl acetate, layered, the water phase was extracted twice with ethyl acetate, the organic phases were combined, dried, separated by silica gel column chromatography, eluted with MeOH:CH2Cl2=1:30, yield 46 g of II1.

1. waitthe reaction was performed at 100° C. for 8 h
2. temperaturecooled
3. distillationdistilled at a reduced pressure
4. customto remove DMF
5. additionadded with water and ethyl acetate
6. extractionthe water phase was extracted twice with ethyl acetate
7. customdried
8. customseparated by silica gel column chromatography
9. washeluted with MeOH