関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Heptanamine | HCID 8127 | — |
| 反応物 | Delta-Valerolactone | HCID 10953 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Pentanamide, N-heptyl-5-hydroxy- | HCID 10262728 | 95% |
反応手順
Delta valerolactone (40 g, 0.4 mole) was added dropwise with stirring to n-heptylamine (50.6 g, 0.4 mole) so that the temperature of the mixture was maintained at 85° to 90° C. Heat was applied and the temperature raised to 110° C. over 20 minutes after which the temperature was maintained at 110° to 115° C. for a further 6 hours (after 3 hours N.M.R. indicated that the reaction was 90 to 95% complete). Toluene (200 ml, 173 g) was added and the solution cooled to 0° C. with stirring. After 1 hour at 0° C., the solid was collected and washed successively with ice cold toluene (50 ml, 43 g) and n-heptane (50 ml, 34 g). The material was dried at room temperature overnight to give the product. (81.6 g (95% yield) m.p. 53° to 54° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05212318 |
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| 出典データセット | uspto-grants-1993_05 |
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| ORD ID | ord-a2db769c74e14bb0bf039bde9917aa5b |
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| 出典メモ | uspto-grants-1993_05 |
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