反应详情

温度

105 °C

6-Chloro-2-iodo-9-isopropyl-9H-purine (1.7 g, 5.2 mmol), [(4-amino-phenyl)-ethoxy-phosphinoylmethyl]-phosphonic acid diethyl ester (2.6 g, 7.7 mmol), and DIPEA (2.7 mL, 15.5 mmol) were dissolved in EtOH (27 mL) and heated in a sealed tube at 105° C. for 48 h. After cooling, the EtOH was evaporated. The residue was poured into water and extracted with EtOAc. The combined extracts, were washed with water, sat'd NaCl, then dried over MgSO4 and filtered. Concentration yielded an oil which was purified by silica gel chromatography (11% MeOH/EtOAc) to a glassy solid (1.8 g, 53%): MS [M+H]+ 621.

1. temperatureAfter cooling
2. customthe EtOH was evaporated
3. additionThe residue was poured into water
4. extractionextracted with EtOAc
5. washThe combined extracts, were washed with water
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationConcentration
9. customyielded an oil which
10. customwas purified by silica gel chromatography (11% MeOH/EtOAc) to a glassy solid (1.8 g, 53%)