化工社化工社 化学情報印刷レポート · 研究参考用
Water → (8-Methyl-1,4-dioxaspiro(4.5)decan-8-yl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | Methyl 8-methyl-1,4-dioxaspiro[4.5]decane-8-carboxylate | HCID 22591390 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | (8-Methyl-1,4-dioxaspiro(4.5)decan-8-yl)methanol | HCID 12568263 | 89.9% |
反応手順
The thus-obtained methyl 4,4-ethylenedioxy-1-methylcyclohexanecarboxylate (37.8 g) was dissolved in ether (100 ml), and the solution was added dropwise to a refluxing suspension of LiAlH4 (6.7 g) in ether (400 ml). After the addition, the mixture was stirred at room temperature for an hour and then cooled with ice. Ethyl acetate (20 ml) and then water (35 ml) were added dropwise cautiously thereto. The solid precipitate was filtered off, and the filtrate was distilled under reduced pressure to give 4,4-ethylenedioxy-1-methylcyclohexanemethanol (29.5 g, 89.9% yield, b.p. 120°-125° C./0.5 mmHg, m.p. 42°-43° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04461902 |
| 出典データセット | uspto-grants-1984_07 |
| ORD ID | ord-6dd396102f7743449c6ca1724ade3805 |
| 出典メモ | uspto-grants-1984_07 |