反应详情

温度

60 °C

A mixture of 2-butoxy-8-methoxy-9H-purin-6-amine trifluoroacetate salt (223 mg) and potassium carbonate (264 mg) in dry DMF (2 mL) were heated at 60° C. under nitrogen with stirring for 1 h. 4-(Bromomethyl)-2,2-dimethyltetrahydro-2H-pyran (158 mg) was added and the reaction was stirred for 16 h at 60° 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 a brown oil. The crude material was purified by normal phase chromatography (ISCO) using 5-20% methanol/EtOAc as eluent to give a pale oil (181 mg). The material was re-purified by normal phase chromatography (ISCO) using 0-15% methanol/EtOAc as eluent to give the title compound (161 mg).

1. stirringthe reaction was stirred for 16 h at 60° C
2. customThe mixture was quenched with water
3. extractionextracted with EtOAc (×3)
4. washThe combined organics were washed with water and brine
5. customdried
6. customevaporated
7. customto give a brown oil
8. customThe crude material was purified by normal phase chromatography (ISCO)