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Water → 2-Methylpyrimidine-5-carbaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Acetamidine monohydrochloride | HCID 67170 | — |
| 反応物 | Vinamidinium | HCID 101612644 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Methylpyrimidine-5-carbaldehyde | HCID 3160970 | — |
反応手順
To a stirred slurry of acetamidine hydrochloride (19.4 g, 0.20 mol) and vinamidinium salt (48.91 g, 0.183 mol) in acetonitrile (240 mL) was added a solution of 40% wt. NaOH in water (27.4 g, 0.274 mol) over a 30 minutes period. After the addition was complete, the resulting reaction mixture was stirred at room temperature overnight. The mixture was concentrated in vacuo and diluted with water (250 mL) and extracted with EtOAc (3×250 mL). The combined organic layers were dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel chromatography (0-100% EtOAc/hexanes) to afford a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653091B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-79f8da4c72524c5b974fbac6a46a4b0b |
| 出典メモ | uspto-grants-2014_02 |