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Ethylene Glycol → Methyl 1,4-dioxaspiro[4.5]decane-8-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Methyl 4-oxocyclohexanecarboxylate | HCID 226643 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Methyl 1,4-dioxaspiro[4.5]decane-8-carboxylate | HCID 10845708 | — |
反応手順
To a solution of 8 g (0.51 mole) of methyl 4-oxocyclohexane-1-carboxylate in 50 ml of dry benzene is added 4 g (0.064 mole) of ethylene glycol and 0.10 g of p-toluenesulfonic acid and this mixture is refluxed overnight with a Dean-Stark apparatus. The cooled reaction is allowed to stand and the bottom layer (ethylene glycol) separated and the remaining benzene layer washed with aqueous sodium bicarbonate, dried over MgSO4, and stripped to dryness, giving methyl 1,4-dioxaspiro[4,5]decane-8-carboxylate as a clear liquid residue. This material is used without further purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05385912 |
| 出典データセット | uspto-grants-1995_01 |
| ORD ID | ord-02882bd1f8074dc698cb04586b0b5eb5 |
| 出典メモ | uspto-grants-1995_01 |