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 | 2-tert-Butyloxirane | HCID 92174 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(2-Hydroxy-3,3-dimethylbutoxy)-isoindole-1,3-dione | HCID 21111533 | 14% |
反応手順
To a solution of 3,3-dimethyl-1,2-epoxybutane (5.0 mL, 41.0 mmol) in DMF (100 mL) was added N-hydroxyphthalimide (8.03 g, 49.2 mmol) and triethylamine (6.90 mL, 49.2 mmol). The solution was heated at 75° C. for two days. The solution was cooled to room temperature, diluted with ethyl acetate and washed with water (2×), saturated potassium carbonate (3×), brine (2×), dried over Na2SO4 and concentrated to an orange solid. Purification using flash column chromatography (dichloromethane) provided the desired product as a white solid (1.50 g, 14%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07538120B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-12fc7a23402c426d90a0a122f4dec1e0 |
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| 出典メモ | uspto-grants-2009_05 |
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