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Diethyl Ether → Methyl 6-oxohexanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | HCID 178418287 | HCID 178418287 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 6-oxohexanoate | HCID 81164 | 60% |
反応手順
The foregoing crude product was dissolved in CH2Cl2 (300 mL). Sodium acetate (2.6 g, 32 mmol) and PCC (32.7 g, 50 mmol) was added. After being stirred at room temperature for 2 h, ether (2000 mL) was added, the reaction mixture was filtered through Florisil, and the filtrate was concentrated. The residue was distilled at reduced pressure (80–84° C. at 0.2 mmHg) to give 6-oxo-hexanoic acid methyl ester (8.58 g, 60%) as a colorless oil: 1H NMR (300 MHz, CDCl3) δ 9.72 (1H, t, J=1.5 Hz), 3.62 (3H, s), 2.43 (2H, m), 2.29 (2H, m), 1.62 (4H, m); 13C NMR (75 MHz, CDCl3) δ 201.99, 173.64, 51.73, 43.66, 33.88, 24.53, 21.69.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091357B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-0e8fb063cff74ebcb0d4c77b40a93c43 |
| 出典メモ | uspto-grants-2006_08 |