化工社化工社 化学情報印刷レポート · 研究参考用
Water → Ethyl 2-(4,4-dimethyl-2-cyclohexen-1-ylidene)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethyl phosphonoacetate | HCID 13345 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Cyclohexen-1-one, 4,4-dimethyl- | HCID 136839 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 2-(4,4-dimethyl-2-cyclohexen-1-ylidene)acetate | HCID 53954530 | 100% |
反応手順
To a suspension of sodium hydride (60% dispersion in oil, 2.2 g, 55 mmol) in tetrahydrofuran (100 ml) at 0° C. was added ethyl 2-(diethoxyphosphoryl)acetate (11.2 g, 50 mmol) over 30 min, and the mixture was stirred at room temperature for 1 h. To this was added 4,4-dimethyl-2-cyclohexene-1-one over 20 min and the reaction mixture was stirred for a further 1 h. Water (100 ml) was added and the mixture was extracted with ether (2×100 ml). The combined extracts were dried (MgSO4), filtered and concentrated in vacuo to afford the title compound as a colourless oil (9.7 g, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06610711B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-0ffd96e046f24d81b30dca21d1f9a2bc |
| 出典メモ | uspto-grants-2003_08 |