反应详情

To a solution of 8-bromo-2-chloro-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purin-6-amine (1.36 g) in dry MeOH (27.5 mL) was added 1M sodium hydroxide solution (27.5 mL) and the mixture was stirred at reflux for 30 mins. The reaction was cooled to room temperature and concentrated in vacuo. The residue obtained was triturated with water (60 mL) and extracted with EtOAc (120 mL). The organic layer was washed with brine (60 mL), dried over MgSO4, filtered and concentrated in vacuo to give a pink/white solid. The material was taken up in MeOH/DMSO (1:1) and a precipitate crashed out of solution. The solid was filtered off and the filtrate was purified by C18 reverse phase chromatography (ISCO) using water (0.1% formic acid)-acetonitrile (0.05% formic acid) as eluent (10-45%). The filtered solid was combined with the material obtained from the purification to give the title compound (192 mg).

1. temperatureat reflux for 30 mins
2. concentrationconcentrated in vacuo
3. customThe residue obtained
4. customwas triturated with water (60 mL)
5. extractionextracted with EtOAc (120 mL)
6. washThe organic layer was washed with brine (60 mL)
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customto give a pink/white solid
11. filtrationThe solid was filtered off
12. customthe filtrate was purified by C18 reverse phase chromatography (ISCO)
13. customobtained from the purification