関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isobutyl iodide | HCID 10556 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-(4-Nitrophenyl)-3-azabicyclo[3.1.1]heptane-2,4-dione | HCID 14872629 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Isobutyl-1-(4-nitrophenyl)-3-azabicyclo[3.1.1]heptane-2,4-dione | HCID 14872630 | — |
反応手順
0.36 g of sodium hydride is added to a solution of 2.46 g of 1-(4-nitrophenyl)-3-azabicyclo[3.1.1]heptane-2,4-dione in 25 ml of N,N-dimethylformamide and the whole is stirred at room temperature for 30 minutes. 2.76 g of isobutyl iodide dissolved in 10 ml of N,N-dimethylformamide are then added dropwise thereto. When the reaction is complete, the reaction mixture is freed of N,N-dimethylformamide. The residue is partitioned between ethyl acetate and water, and the organic phase is dried over magnesium sulphate and, after concentration by evaporation and purification by chromatography over silica gel in the system ethyl acetate/hexane 1:2, the product is obtained in the form of a solid. Melting point 136°-137°. Rf (ethyl acetate/hexane 4:1)=0.6.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04677129 |
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| 出典データセット | uspto-grants-1987_06 |
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| ORD ID | ord-dc11d1a307d54ef491e70b9463a852cc |
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| 出典メモ | uspto-grants-1987_06 |
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