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Ethylene Glycol → 2-(3-Chloropropyl)-2-phenyl-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 | Toluene | HCID 1140 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 4-Chlorobutyrophenone | HCID 253533 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(3-Chloropropyl)-2-phenyl-1,3-dioxolane | HCID 12866338 | — |
反応手順
A mixture of γ-chlorobutyrophenone (33.2 g; 0.182 mol), ethylene glycol (20.3 ml; 0.363 mol), p-toluenesulfonic acid (a pinch) and toluene (300 ml) is heated at reflux for 40 hours, and the water formed in the reaction is azeotroped off. After 20 hours, more ethylene glycol (20.3 ml; 0.363 mol) is added. On completion of the reaction the mixture is extracted with saturated aqueous sodium bicarbonate solution (300 ml), the organic layer is washed with 1 N sodium hydroxide solution and then with water, and is evaporated to afford 37.0 g of a cream colored solid, m.p. 54°-55.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04294986 |
| 出典データセット | uspto-grants-1981_10 |
| ORD ID | ord-be9f57e079234de7b59a4a89c743a87c |
| 出典メモ | uspto-grants-1981_10 |