反应详情

温度

0 °C

To a cooled flask (0° C.) under an atmosphere of N2 containing 0.096 g (4.02 mmol) of sodium hydride was added 2.0 mL of absolute ethanol. After the effervescence had ceased, the solution was transferred via pipette to a cooled (0° C.) pressure flask, under an atmosphere of N2, containing a mixture of [(4-{2-Fluoro-9-[2-(3-hydroxy-phenyl)-ethyl]-9H -purin-6-ylamino}-phenyl)-hydroxy-phosphinoylmethyl]-phosphonic acid (0.199 g, 0.39 mmol) in 2.0 mL of absolute ethanol. Upon sealing the reaction vessel, the resulting mixture was stirred at ambient temperature for ˜10 min, then heated at 80° C. overnight. Ethanol was removed via N2 flow (slight heat) and the resulting thick suspension was dissolved in 25 mL of H2O (adjusted to pH ˜8 with 10% NaOH), filtered (0.2 μm, PTFE filter), and purified by RP-HPLC (CH3CN/H2O). Lyophilization provided a white solid (0.105 g): m/z 532 (M−H).

1. additionunder an atmosphere of N2, containing
2. temperatureheated at 80° C. overnight
3. customEthanol was removed via N2
4. temperature(slight heat)
5. dissolutionthe resulting thick suspension was dissolved in 25 mL of H2O (adjusted to pH ˜8 with 10% NaOH)
6. filtrationfiltered
7. filtration(0.2 μm, PTFE filter)
8. custompurified by RP-HPLC (CH3CN/H2O)