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Ethylene Glycol → 2-(3-Methylthiophen-2-yl)-1,3-dioxolane
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 | 3-Methyl-2-thiophenecarboxaldehyde | HCID 79911 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(3-Methylthiophen-2-yl)-1,3-dioxolane | HCID 12926522 | — |
反応手順
A mixture of 3-methylthiophene carboxaldehyde (6.8 g), ethylene glycol (10 ml) and p-toluenesulfonic acid (0.30 g) in toluene (125 ml) was heated at reflux for 18 hours. The reaction mixture was cooled; extracted with 2M aqueous sodium carbonate and then dried with brine and over magnesium sulfate. Analysis of the crude product indicated that the reaction was incomplete so the crude material was re-subjected to the ketalisation conditions as outlined above. The crude material isolated after reprocessing was distilled under reduced pressure (1 mmHg) to give the title compound as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091237B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-74b822405f8e419aaae0449610e9ed3b |
| 出典メモ | uspto-grants-2006_08 |