反应详情

A suspension of 2-amino-6-chloro-9-(2,3,5-tri-O-acetyl-β-D-ribofuranosyl)purine (291.2 g, 0.68 mol, Example 1, Step B) in 2-propanol and water (1:1, 15,560 mL) which was heated to achieve homogeneity. The solution was cooled to <15° C. and then t-butyl nitrite (357 mL, 3.0 mol) was added. The reaction was allowed to warm to room temperature and stirred until the evolution of gas subsided. The reaction was partitioned between ethyl acetate (7,300 mL) and water and the phases allowed to separate. The aqueous layer was further extracted with ethyl acetate (2×7,300 mL) and the combined organic layers were dried over magnesium sulfate, filtered and removed under reduced pressure to yield a viscous oil. Typical Yield: Quantitative.

1. temperaturewas heated
2. temperatureThe solution was cooled to <15° C.
3. customThe reaction was partitioned between ethyl acetate (7,300 mL) and water
4. customto separate
5. extractionThe aqueous layer was further extracted with ethyl acetate (2×7,300 mL)
6. dry with materialthe combined organic layers were dried over magnesium sulfate
7. filtrationfiltered
8. customremoved under reduced pressure
9. customto yield a viscous oil