関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetate | HCID 175 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Isoamyl Alcohol | HCID 31260 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Isoamyl Acetate | HCID 31276 | — |
反応手順
1-Butanol, 3 methyl, acetate. Under an atmosphere of argon, acetyl chloride (6.5 ml, 91.8 mmol) was added dropwise to a 0° C. solution of isoamyl alcohol (5 ml, 45.9 mmol), N, N-dimethylpyridine (2.8 g, 23 mmol), and anhydrous pyridine (4.1 ml, 50.5 mol) in dichloromethane (92 ml). The reaction mixture was poured into 100 ml of 0.1 N HCl, and the resulting layers were separated. The organic layer was washed with 50 ml of saturated aqueous ammonium chloride then dried over magnesium sulfate. The organic layer was filtered and concentrated in vacuo to a clear oil. The resulting oil was purified by distillation (bp 134-136° C.) to give isoamyl acetate. 1H NMR (300 MHz, CDCl3) 4.08 (t, 2H, J 6.9), 2.03 (s, 3H), 1.68 (m, 1H), 1.51 (q, 2H, J 6.9), 0.92 (d, 6H, J 6.6).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06911338B2 |
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| 出典データセット | uspto-grants-2005_06 |
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| ORD ID | ord-2213bafc23154883acb230183da6cb34 |
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| 出典メモ | uspto-grants-2005_06 |
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