反应详情

2,2′-Anhydro-5-methyluridine (195 g, 0.81 M) tris(2-methoxyethyl)borate (231 g, 0.98 M) and 2-methoxyethanol (1.2 L) were added to a 2 L stainless steel pressure vessel and placed in a pre-heated oil bath at 160° C. After heating for 48 hours at 155-260?C., the vessel was opened and the solution evaporated to dryness and triturated with MeOH (200 mL). The residue was suspended in hot acetone (1 L). The insoluble salts were filtered, washed with acetone (150 mL) and the filtrate evaporated. The residue (280 g) was dissolved in CH3CN (600 mL) and evaporated. A silica gel column (3 kg) was packed in CH2C2/acetone/MeOH (20:5:3) containing 0.5% Et3NH. The residue was dissolved in CH2Cl2 (250 mL) and adsorbed onto silica (150 g) prior to loading onto the column. The product was eluted with the packing solvent to give 160 g (63%) of product.

1. customplaced in a pre-heated oil bath at 160° C
2. temperatureAfter heating for 48 hours at 155-260?C
3. customthe solution evaporated to dryness
4. customtriturated with MeOH (200 mL)
5. filtrationThe insoluble salts were filtered
6. washwashed with acetone (150 mL)
7. customthe filtrate evaporated
8. dissolutionThe residue (280 g) was dissolved in CH3CN (600 mL)
9. customevaporated
10. additioncontaining 0.5% Et3NH
11. dissolutionThe residue was dissolved in CH2Cl2 (250 mL)
12. washThe product was eluted with the packing solvent