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Methanol → HCID 22672509、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Cyanoethyl N,N-diisopropylchlorophosphoramidite | HCID 2734844 | — |
| 反応物 | HCID 22672512 | HCID 22672512 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 22672509 | HCID 22672509 | 65.2% |
反応手順
To a solution of 33a (0.6 g, 1.5 mmol) in 10 mL of anhydrous CH2Cl2 was added triethylamine (0.4 mL) followed by 2-cyanoethyl diisopropylchlorophosphoramidite (0.35 mL, 1.6 mmol). The solution was kept at room temperature for 1 h and treated with 0.1 mL of MeOH. The solvent was evaporated and the residue was partitioned between ethyl acetate and saturated NaHCO3. The organic phase was washed with saturated NaCl, dried over Na2SO4 and concentrated. The crude product was chromatographed on silica eluting with 5% triethylamine in ethyl acetate. Concentration of the pure product fractions and drying under vacuum afforded 0.59 g (65%) of 34 as a colorless, viscous oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699975B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-b1a39229bce144ebaf40e061ad6191e9 |
| 出典メモ | uspto-grants-2004_03 |