関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N-Hydroxyphthalimide | HCID 10665 | — |
| 反応物 | Picolyl chloride hydrochloride | HCID 23392 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(Pyridin-2-ylmethoxy)-isoindole-1.3-dione | HCID 12213945 | 46% |
反応手順
2-Chloromethylpyridine hydrochloride (514 mg, 3.13 mmol), N-hydroxyphthalimide (515 mg, 3.18 mmol), and triethylamine (1.3 mL, 9.3 mmol) were mixed in acetonitrile (5 mL) and stirred at 80° C. for 2.5 hours. The reaction mixture was diluted with ethyl acetate and washed sequentially with 1N NaOH(aq), water, and brine. The organic phase was dried over MgSO4, filtered, and concentrated. The residue was recrystallized from ethyl acetate and hexanes to provide N-(pyridine-2-ylmethoxy)phthalimide (364 mg, 1.44 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524764B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-a0c6c07c91f64f5fb80b8604da9ff8f9 |
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| 出典メモ | uspto-grants-2013_09 |
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