反应详情

The compound (480 mg, 0.71 mmol) prepared in Example 24 was dissolved in dried acetonitrile (2 mL). To the solution was added 2-cyanoethoxy N,N,N′,N′-tetraisopropylphosphorodiamidite (343 μL, 1.07 mmol) dissolved in dried acetonitrile (2 mL) and then diisopropylammonium 1H-tetrazolide (92 mg, 0.54 mmol), followed by vigorous stirring at room temperature for 15 hours. The reaction was terminated with a small amount of water, and then the reaction system was concentrated under reduced pressure, diluted with chloroform, and washed with saturated brine. The organic layer was dried with anhydrous sodium sulfate, and filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography eluting with chloroform:methanol:triethylamine (98:1.5:0.5) to give the title compound (300 mg, 0.34 mmol).

1. customThe reaction was terminated with a small amount of water
2. concentrationthe reaction system was concentrated under reduced pressure
3. additiondiluted with chloroform
4. washwashed with saturated brine
5. dry with materialThe organic layer was dried with anhydrous sodium sulfate, and filtrate
6. concentrationwas concentrated under reduced pressure
7. washeluting with chloroform:methanol:triethylamine (98:1.5:0.5)