関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5'-O-(4,4'-Dimethoxytrityl)-2'-O-[2-(N-methylcarbamoyl)ethyl]-4-N-acetylcytidine | HCID 53253292 | — |
| 反応物 | 2-cyanoethoxy N,N,N',N'-tetraisopropylphosphorodiamidite | HCID 86638306 | — |
| 反応物 | HCID 178458033 | HCID 178458033 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 178485724 | HCID 178485724 | 63% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08039611B2 |
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| 出典データセット | uspto-grants-2011_10 |
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| ORD ID | ord-daea591bed8c44648f844e41ec12ab51 |
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| 出典メモ | uspto-grants-2011_10 |
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