反应详情

温度

60 °C

A mixture of N2-Butyl-8-methoxy-9H-purine-2,6-diamine trifluoroacetic acid salt (200 mg) and potassium carbonate (236 mg) in dry DMF (2 mL) were heated at 60° C. under nitrogen with stirring for 1 h. (2,2-Dimethyltetrahydro-2H-pyran-4-yl)methyl methanesulfonate (152 mg) was added and stirring was continued for 5 h at 50° C. The reaction was cooled to room temperature and stirred for 16 h. Lithium bromide (50 mg) was added and heating was continued for 5 h at 50° C., then 8 h at 90° C. The mixture was quenched with water and extracted with EtOAc (×3). The combined organics were washed with water and brine, dried using a hydrophobic frit and evaporated to give crude material (210 mg). This was purified by C18 reverse phase chromatography (ISCO) using water (0.1% formic acid)-acetonitrile (0.05% formic acid) as eluent (20-60%) to give the title compound (75 mg).

1. additionwas added
2. temperatureThe reaction was cooled to room temperature
3. stirringstirred for 16 h
4. temperatureheating
5. waitwas continued for 5 h at 50° C.
6. custom8 h
7. customat 90° C
8. customThe mixture was quenched with water
9. extractionextracted with EtOAc (×3)
10. washThe combined organics were washed with water and brine
11. customdried
12. customevaporated
13. customto give crude material (210 mg)
14. customThis was purified by C18 reverse phase chromatography (ISCO)