反应详情

温度

50 °C

To a stirred solution of 2',3'-dideoxy-3'-fluorouridine (1 g, 4.34 mmoles) in dry pyridine (25 ml) at 0° C. was slowly added freshly distilled p-toluoyl chloride (0.63 ml, 4.78 mmoles). After the addition was complete, the mixture was stirred at 50° C. for 1.5 hrs., cooled and the solvent removed under reduced pressure. The residue was dissolved in chloroform (35 ml) and the solution extracted with 1M sulphuric acid (2×20 ml), water (2×30 ml) and dried (sodium sulphate). Evaporation of the solvent and purification of the residue by silica column chromatography eluting with 5% MeOH/CH2Cl2 afforded the title compound.

1. additionAfter the addition
2. temperature, cooled
3. customthe solvent removed under reduced pressure
4. dissolutionThe residue was dissolved in chloroform (35 ml)
5. extractionthe solution extracted with 1M sulphuric acid (2×20 ml), water (2×30 ml)
6. dry with materialdried (sodium sulphate)
7. customEvaporation of the solvent and purification of the residue by silica column chromatography
8. washeluting with 5% MeOH/CH2Cl2