関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | 1-Adamantaneacetyl chloride | HCID 2771882 | — |
| 反応物 | 5-amino-1H-isochromen-1-one | HCID 10080666 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-adamantan-1-yl-N-(1-oxo-1H-isochromen-5-yl)-acetamide | HCID 59752015 | 91.3% |
反応手順
To a solution of 5-amino-1H-isochromen-1-one (2.95 g, 18.3 mmol) and NMM (2.02 mL, 18.3 mmol) in 1,4 dioxane (55 mL) was added dropwise at room temperature a solution of 1-adamantaneacetic acid chloride (3.9 g, 18.3 mmol) in 1,4-dioxane (40 mL). The reaction mixture was stirred at room temperature for 3 h and then partitioned between DCM (400 mL) and water (200 mL). The layers were separated. The aqueous phase was washed with DCM (100 mL). The combined organic layers were dried over sodium sulfate, filtered and evaporated. The crude product was suspended in hexane (100 mL) and filtered off. The solid was collected on the filter and dried in vacuo to yield 2-adamantan-1-yl-N-(1-oxo-1H-isochromen-5-yl)-acetamide as a yellow solid (5.6 g, 16.7 mmol, 91%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07402596B2 |
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| 出典データセット | uspto-grants-2008_07 |
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| ORD ID | ord-ab2f41996fd24e61be44dae0e8627aab |
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| 出典メモ | uspto-grants-2008_07 |
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