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Ethylene Glycol → 6-Methyl-1,4-dioxospiro[4.5]decane-6-propionic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Methyl 3-(1-methyl-2-oxocyclohexyl)propanoate | HCID 574325 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 6-Methyl-1,4-dioxospiro[4.5]decane-6-propionic acid methyl ester | HCID 54458722 | — |
反応手順
A solution of 1-methyl-2-oxocyclohexanepropionic acid methyl ester (96.1 g, 0.48 mole), described in Example 6, ethylene glycol (100 ml) and p-toluenesulfonic acid (2.0 g) in dry benzene (1600 ml) is heated at reflux for 6 hr using a water separator. The benzene solution is cooled, washed with saturated aqueous sodium bicarbonate solution (2 × 100 ml) then brine (2 × 100 ml), dried (MgSO4) and concentrated to yield the title compound as an oil, ν maxCHCl3 1725, 1085 cm-1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04057559 |
| 出典データセット | uspto-grants-1977_11 |
| ORD ID | ord-c73c0e10c4f24e459151ea5a2f68d76c |
| 出典メモ | uspto-grants-1977_11 |