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Methyl iodide → 3,6-Dimethylheptane-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,4-Heptanedione, 6-methyl- | HCID 76354 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3,6-Dimethylheptane-2,4-dione | HCID 538283 | 94% |
反応手順
To 0.1 mol sodium hydride was added 100 ml anhydrous tetrahydrofuran, then added slowly dropwise 0.1 mol 6-methyl-2,4-heptandione at room temperature. The reaction was stirred for 0.5 hours, then 0.12 mol iodomethane was added dropwise and the reaction was stirred at room temperature for further 10 hours. Upon completing the reaction, 20 ml water was added. The mixture was extracted with ethyl acetate. After removing the solvent, distillation under reduced pressure gave a cut fraction 88-9° C./1 kPa (165-166° C. at atmosphere pressure), and the yield was 94%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07388061B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-bd5b8d7ad93241e686914bdcd1e363f5 |
| 出典メモ | uspto-grants-2008_06 |