反应详情

(3aS,4S,6R,6aR)-6-(6-Chloro-purin-9-yl)-2,2-dimethyl-tetrahydro-furo[3,4-d][1,3]dioxole-4-carboxylic acid (2.5 g) suspended in 1,2-dimethoxymethane (100 ml) was treated with 2,2-dimethyl-propionic acid hydrazide (1.1 g) and 2-ethoxy-1-ethoxycarbonyl-1,2-dihydroquinoline (EEDQ), and the mixture heated under reflux for 16 h. The mixture was poured into aqueous citric acid (250 ml) and extracted with ethyl acetate; the organic layers were washed with citric acid and brine, dried (MgSO4) and evaporated in vacuo to give the crude product. Purification by flash chromatography on silica gel (Biotage cartridge), eluting with ethyl acetate:cyclohexane 65:35, gave the title compound as a white solid (1.92 g).

1. temperaturethe mixture heated
2. temperatureunder reflux for 16 h
3. extractionextracted with ethyl acetate
4. washthe organic layers were washed with citric acid and brine
5. dry with materialdried (MgSO4)
6. customevaporated in vacuo
7. customto give the crude product
8. customPurification by flash chromatography on silica gel (Biotage cartridge)
9. washeluting with ethyl acetate:cyclohexane 65:35