化工社化工社 化学情報印刷レポート · 研究参考用
Ethylene Glycol → Methyl 1,4-dioxaspiro[4.5]decane-7-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| 反応物 | Methyl 3-oxocyclohexane-1-carboxylate | HCID 566099 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl 1,4-dioxaspiro[4.5]decane-7-carboxylate | HCID 372311 | — |
反応手順
Methyl 3-oxocyclohexanecarboxylate (930 mg) and pyridinium p-toluenesulfonate (299 mg) were combined in toluene (29.8 mL) to give a colorless solution. Ethylene glycol (0.996 mL) was added and the reaction was refluxed under Dean-Stark conditions for 2 days. The reaction was cooled to room temperature, triethylamine was added, and then the mixture was concentrated by rotary evaporation. The residue was purified by regular phase flash column chromatography (Analogix 0-40% hexane/ethyl acetate).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09034875B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-89ae61a478bb4ddc8bfe5bc0a9a34275 |
| 出典メモ | uspto-grants-2015_05 |