化工社化工社 化学情報印刷レポート · 研究参考用
Toluene → 5-Isopropyl-1,3-dimethyl-bicyclo[3.2.1]oct-3-en-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Ethylaluminum dichloride | HCID 11237 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2,6-Dimethyl-6-(3-methyl-but-2-enyl)-cyclo-hex-2-enone | HCID 11579258 | — |
| 生成物 | 5-Isopropyl-1,3-dimethyl-bicyclo[3.2.1]oct-3-en-2-one | HCID 45098702 | 90% |
反応手順
To a solution of 2,6-dimethyl-6-(3-methyl-but-2-enyl)-cyclohex-2-enone (5.00 g, 26.04 mmol) in toluene (40 ml) was added dropwise neat EtAlCl2 (97%, 1.5 eq., 4.96 g, 39.06 mmol). During the addition, the temperature was kept below 10° C. The brown mixture was kept at room temperature over night and was then poured on icecold saturated NH4Cl. The mixture was extracted with MTBE, washed with brine, dried (MgSO4) and concentrated in vacuo. The residue was distilled bulb to bulb to yield 4.50 g (90%) of an colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07691802B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-46c8f7c24d3c44b4b8e49d55ad04b40d |
| 出典メモ | uspto-grants-2010_04 |