化工社化工社 化学情報印刷レポート · 研究参考用
Gamma-Butyrolactone → 1,3-Dioxo-6-hydroxy-1(3'-tert-butyl-phenyl)-hexane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Gamma-Butyrolactone | HCID 7302 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-(3-tert-Butylphenyl)ethan-1-one | HCID 13657978 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1,3-Dioxo-6-hydroxy-1(3'-tert-butyl-phenyl)-hexane | HCID 57839120 | — |
反応手順
To a stirring suspension of NaH (60% in oil, 7.66 g) in ether (480 ml) at 0° C. was added ethanol (479 μL), followed by γ-butyrolactone (6.18 ml). This was followed by dropwise addition of 1-(3-tert-butyl-phenyl)-ethanone (13.5 g) in ether (80 ml). The resulting mixture was allowed to warm to room temperature and stirred for 72 hours. After careful addition of ethanol (10.5 ml), ammonium chloride solution (10 g in 250 ml water) was then added, ether layer was then separated and washed with brine (300 ml), dried over MgSO4 and concentrated in vacuo to give 1,3-dioxo-6-hydroxy-1(3′-tert-butyl-phenyl)-hexane as crude product (18.5 g). This required no purification and was immediately used in the next reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07589095B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-44a0741dc5894e7abf0078fe50f4a301 |
| 出典メモ | uspto-grants-2009_09 |