反应详情

To a mixture of 5-fluorouracil (0.85 g, 6.54 mmol) and compound 2 (3.0 g, 5.94 mmol) in anhydrous MeCN (100 ml) were successively added HMDS (1.25 ml, 5.95 mmol), ClSiMe3 (0.6 ml, 4.76 mmol) and SnCl4 (0.83 ml, 7.13 mmol). The resulting clear solution was refluxed for 1 hour when TLC indicated completion of the reaction. The solvent was evaporated and the residue dissolved in EtOAc (250 ml), washed with NaHCO3 and H2O. The EtOAc layer was dried, filtered and evaporated to give a white solid and it was crystallized from CHCl3 /MeOH (1-2%) to give compound 5 (2.11 g, 61.9%) as white crystals: m.p. 208°-209° C.

1. temperatureThe resulting clear solution was refluxed for 1 hour when TLC
2. customcompletion of the reaction
3. customThe solvent was evaporated
4. dissolutionthe residue dissolved in EtOAc (250 ml)
5. washwashed with NaHCO3 and H2O
6. dry with materialThe EtOAc layer was dried
7. filtrationfiltered
8. customevaporated
9. customto give a white solid and it
10. customwas crystallized from CHCl3 /MeOH (1-2%)