反应详情

温度

50 °C

To 500 mL of an aqueous pH 6.0, 50 mM citrate buffer, prepared as described in Example 2c, was added 2-amino-6-dimethylaminopurine (0.0891 g, 0.5 mmol) and 3'-azido-3'-deoxythymidine (0.668 g, 2.5 mmol). Solution was achieved by heating the mixture at 50° C. with sonication. A sample was removed as a control. A 24 mL solution of trans-N-deoxyribosylase (Example 2b) at an activity of 1400 units/mL was added. The reaction was heated at 50° C. Seven days later 0.0891 g, 0.5 mmol, of 2-amino-6-dimethylamino purine was added to the reaction. The reaction was terminated after fourteen days. The reaction was heated to 80° C. to precipitate the enzyme and then filtered. The aqueous solution was extracted with ethyl acetate to remove the product. The combined ethyl acetate fractions were dried with magnesium sulfate, filtered, and the solvent was removed in vacuo to give a foam. The foam was chromatographed on 90 g of silica gel eluted with chloroform/methanol (97:3, v/v). Chromatography a second time on silica gel (230-400 mesh) eluted with chloroform/methanol (98:2, v/v) gave pure product. The product containing fractions were combined and the solvents removed in vacuo to give the product as a solid (41% yield).

1. customwith sonication
2. customA sample was removed as a control
3. additionA 24 mL solution of trans-N-deoxyribosylase (Example 2b) at an activity of 1400 units/mL was added
4. temperatureThe reaction was heated at 50° C
5. additionSeven days later 0.0891 g, 0.5 mmol, of 2-amino-6-dimethylamino purine was added to the reaction
6. customThe reaction was terminated after fourteen days
7. temperatureThe reaction was heated to 80° C.
8. customto precipitate the enzyme
9. filtrationfiltered
10. extractionThe aqueous solution was extracted with ethyl acetate
11. customto remove the product
12. dry with materialThe combined ethyl acetate fractions were dried with magnesium sulfate
13. filtrationfiltered
14. customthe solvent was removed in vacuo
15. customto give a foam
16. customThe foam was chromatographed on 90 g of silica gel
17. washeluted with chloroform/methanol (97:3
18. washChromatography a second time on silica gel (230-400 mesh) eluted with chloroform/methanol (98:2
19. customv/v) gave pure product
20. additionThe product containing fractions
21. customthe solvents removed in vacuo