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Ethylene Glycol → 1,3-Dioxolane, 2-(3-bromo-4-methylphenyl)-
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 | 3-Bromo-4-methylbenzaldehyde | HCID 816765 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1,3-Dioxolane, 2-(3-bromo-4-methylphenyl)- | HCID 11241979 | 89.1% |
反応手順
11.8 g (60 mmol) of 3-bromo-4-methylbenzaldehyde are placed in 150 ml of toluene in a round-bottomed flask and under nitrogen. 16.5 ml (300 mmol) of ethylene glycol and 571 mg (3 mmol) of para-toluenesulfonic acid are added. The mixture is refluxed for 36 hours and the water formed is separated out using Dean-Stark apparatus. At room temperature, the reaction medium is poured into saturated aqueous sodium hydrogen carbonate solution and then extracted with ether. The organic phase is dried over magnesium sulfate, filtered and evaporated. 13 g (89%) of the expected product are obtained in the form of a brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06924400B2 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-282184698f1f435fb04d2ef09b18096f |
| 出典メモ | uspto-grants-2005_08 |