反应详情

Add to a solution of trans-{4-[6-(1-benzyl-piperidin-4-ylamino)-9-cyclopent-2-enyl-9H-purin-2-ylamino]-cyclohexyl}-carbamic acid tert-butyl ester (8c,1.0-mmol) in 40 mL of methanol, a suspension of Pd black (0.5 wt %) in a small amount of water. Then add a solution of ammonium formate (2.2 mmol) in 10 mL of water, and heat at a gentle reflux overnight. Remove the catalyst by filtration through Celite® and concentrate the filtrate. Dissolve the residue in DCM and extract with water. Remove the white precipitate by filtration through a pad of Celite®, wash the filtrate with brine, dry over sodium sulfate and filter. Concentrate the filtrate and purify the residue on silica gel (50 g) using DCM:methanol (4:1) to give trans-{4-[9-cyclopent-2-enyl-6-(piperidin-4-ylamino)-9H-purin-2-ylamino]-cyclohexyl}-carbamic acid tert-butyl ester (9c.

1. temperatureheat at
2. temperaturea gentle reflux overnight
3. customRemove the catalyst
4. filtrationby filtration through Celite®
5. concentrationconcentrate the filtrate
6. dissolutionDissolve the residue in DCM
7. extractionextract with water
8. customRemove the white precipitate
9. filtrationby filtration through a pad of Celite®
10. washwash the filtrate with brine
11. dry with materialdry over sodium sulfate
12. filtrationfilter
13. concentrationConcentrate the filtrate
14. custompurify the residue on silica gel (50 g)