化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 4-Hydroxy-4-methylcyclohexanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 8-Methyl-1,4-dioxaspiro(4.5)decan-8-ol | HCID 18713075 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Hydroxy-4-methylcyclohexanone | HCID 28539 | 92% |
反応手順
8-Methyl-1,4-dioxaspiro[4.5]decane-8-ol (650 mg, 3.77 mmol) was dissolved in THF (10 ml), followed by addition of 1N aqueous HCl solution (5 ml), and then the resulting mixture was stirred at room temperature for 6 hours. The resulting reaction liquid was concentrated under reduced pressure, and then extracted with 10% MeOH/MC (20 ml×5). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (50% EtOAc/Hexanes), to obtain 443 mg of yellow oil (92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09096571B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-4c8d104f2237465ead45294b8349f757 |
| 出典メモ | uspto-grants-2015_08 |