反应详情

390 mg of 1-phenyl-4,6-dichloropyrazolo[3,4-d]pyrimidine was suspended in 15 ml 95% ethanol. 828 mg norephedrine HCl was dissolved in 100 ml H2O, made basic with 10% KOH, and the free base extracted with 100 ml ether. The organic was dried over MgSO4, filtered, and concentrated to yield an oil which was added to the stirred reaction. After 4 hours the solution became clear and the solvent was removed under vacuum. The crude oil was then purified by radial chromatography (5-10-20% isopropyl alcohol/hexane, 4 mm plate) to yield 535 mg of [R-(S*,R*)]-α-[1-[(1-phenyl-6-chloro-1H-pyrazolo[3,4-d]pyrimidin-4-yl)amino]ethyl]benzenemethanol (90%).

1. extractionthe free base extracted with 100 ml ether
2. dry with materialThe organic was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customto yield an oil which
6. additionwas added to the stirred reaction
7. customthe solvent was removed under vacuum
8. customThe crude oil was then purified by radial chromatography (5-10-20% isopropyl alcohol/hexane, 4 mm plate)