関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-But-3-ynyl-3-(2-chloro-ethyl)-urea | HCID 59787366 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(But-3-yn-1-yl)imidazolidin-2-one | HCID 59787372 | 21% |
反応手順
To a solution of 1-but-3-ynyl-3-(2-chloro-ethyl)-urea (5 g, 28.7 mmol) in THF (100 mL) add tetrabutylammonium bromide (1.82 g, 5.65 mmol) and potassium hydroxide (2.01 g, 35.9 mmol). Heat the resulting suspension at 75° C. for 72 h and allow to cool to room temperature. Dilute the mixture with EtOAc (200 mL), wash with water (2×100 mL) and 1N aqueous HCl (100 mL). Dry the organic phase over MgSO4, filter and concentrate in vacuo to obtain the title compound as a white powder (816 mg, 21%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08420631B2 |
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| 出典データセット | uspto-grants-2013_04 |
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| ORD ID | ord-4cac3a6b517f48ecaaef63dc16fd2ff4 |
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| 出典メモ | uspto-grants-2013_04 |
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