関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Gamma-Butyrolactone | HCID 7302 | — |
| 反応物 | Butylamine | HCID 8007 | — |
| 反応物 | Diisobutylaluminum hydride | HCID 14487 | — |
| 反応物 | N-butyl-4-hydroxybutanamide | HCID 13060238 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-Butanol, 4-(butylamino)- | HCID 20669 | — |
反応手順
A solution of 8.1 g (110 mmol) of n-butylamine and 8.6 g of butyrolactone in 50 ml toluene was allowed to reflux under nitrogen atmosphere for 50 hours. Volatile solvents were removed in vacuo. To a solution of 3.18 gm (20 mmol) of the resultant N-butyl-4-hydroxybutyramide in 50 ml of toluene were added 120 ml (120 mmol) DIBAL(25% W). The solution was heated with stirring at 70° C. for 18 hours. After cooling to 0° C., the reaction was quenched with methanol (113 amount of DIBAL solution was used) followed by addition of saturated solution of Rochelle's salt. The mixture was extracted twice with EtOAc; the organic extracts were washed with brine and dried over Na2SO4.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06946481B1 |
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| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-3e72a5221bb44a03bd5def1130cdaef6 |
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| 出典メモ | uspto-grants-2005_09 |
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