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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 | 4-Chlorobutyrophenone | HCID 253533 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 生成物 | 2-(3-Chloropropyl)-2-phenyl-1,3-dioxolane | HCID 12866338 | 121.2% |
反応手順
A mixture of 36.5 g (0.2 mole) of γ-chlorobutyrophenone, 14 g of ethylene glycol (0.25 mole), 125 ml of toluene, and 0.1 g of p-toluenesulfonic acid is refluxed under a Dean-Stark trap for 1 hr. An additional 4 g of ethylene glycol is added and reflux continued for 3 hrs more. After cooling, the reaction mixture is washed with 5% sodium bicarbonate solution, dried with anhydrous magnesium sulfate, and concentrated. Upon standing at -10° C. overnight, the mixture partially crystallizes. The crystalline product is filtered and washed with petroleum ether to afford 17.7 g of 2-phenyl-2-(3'-chloropropyl)dioxolane, m.p. 56°-58°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04258045 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-6672789bd1dd4593997e3851704b24af |
| 出典メモ | uspto-grants-1981_03 |