反应详情

温度

20 °C

To a solution of (3aS,4S,6R,6aR)-6-(6-chloro-purin-9-yl)-2,2-dimethyl-tetrahydro-furo[3,4-d][1,3]dioxole-4-carboxylic acid (10 g) in dimethylformamide (200 ml) was added 1-hydroxybenzotriazole (3.96 g) and 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (5.62 g). t-Butylacetamidoxime (3.40 g) in dimethylformamide (30 ml) was added and the mixture was stirred at 20° C. for 24 h under nitrogen. The mixture was then heated at 70° C. for a further 36 h. The resulting mixture was then cooled to 20° C., basified with a saturated solution of sodium bicarbonate (200 ml) and extracted with ethyl acetate (2×150 ml). The organic layers were washed with brine (300 ml), dried (MgSO4), evaporated to dryness in vacuo and triturated with ether to give a yellow solid (11.08 g). Purification by chromatography on silica gel, eluting with ethyl acetate:cyclohexane (3:7), afforded the title compound (4.75 g) as a white solid.

1. temperatureThe mixture was then heated at 70° C. for a further 36 h
2. temperatureThe resulting mixture was then cooled to 20° C.
3. extractionextracted with ethyl acetate (2×150 ml)
4. washThe organic layers were washed with brine (300 ml)
5. dry with materialdried (MgSO4)
6. customevaporated to dryness in vacuo
7. customtriturated with ether