反应详情

温度

100 °C

A reactor was charged with 6-chloro-2-[2-(4-chlorophenyl)ethoxy]-9-(2,3,5-tri-O-acetyl-β-D-ribofuranosyl)purine (243.8 g, 0.43 mol, Example 2, Step D) in ethanol (3,660 mL). The reactor was chilled to below −33° C., and ammonia (1500 g) is charged into the reactor. The reactor was sealed, then heated to 100° C. and the reaction was monitored by HPLC. Upon completion (approximately 5 hours), the reactor was cooled, vented, and the contents concentrated under reduced pressure. The crude product is purified by column chromatography eluting with dichloromethane/methanol. The pure fractions were concentrated under reduced pressure to about four liters of solvent and the product collected by vacuum filtration. The off-white solid was washed with dichloromethane and dried in vacuo to yield 82 grams of analytically pure (>99%) product as an off-white solid. Additional fractions were combined to provide an additional 73 g of product of lower purity (90-98%). Combined typical yield: 54%.

1. temperatureThe reactor was chilled to below −33° C.
2. customThe reactor was sealed
3. temperatureUpon completion (approximately 5 hours), the reactor was cooled
4. concentrationthe contents concentrated under reduced pressure
5. customThe crude product is purified by column chromatography
6. washeluting with dichloromethane/methanol
7. concentrationThe pure fractions were concentrated under reduced pressure to about four liters of solvent
8. filtrationthe product collected by vacuum filtration
9. washThe off-white solid was washed with dichloromethane
10. customdried in vacuo