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Benzene → 2,2-Bis-chloromethyl-5,5-dimethyl-1,3-dioxolane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | 1,3-Dichloroacetone | HCID 10793 | — |
| 反応物 | Neopentyl glycol | HCID 31344 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,2-Bis-chloromethyl-5,5-dimethyl-1,3-dioxolane | HCID 68585438 | 34.6% |
反応手順
This compound was synthesized by substantially following the procedure of the above-mentioned article by Isaka, Ejiri, and Nakamura. 69 grams of neopentyl glycol, 76 grams of 1,3-dichloroacetone, 50 ml of benzene, and 2.3 g of p-toluenesulfonic acid were refluxed through a Dean-Stark water separator for 8 hours whereon the reaction was diluted with hexanes and neutralized with aqueous sodium bicarbonate. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo yielding 41.2 g of 2,2-bis-chloromethyl-5,5-dimethyl-1,3-dioxolane, a pale yellow liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741245B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-bd67b92e946446cd96d7efddfc3592d5 |
| 出典メモ | uspto-grants-2010_06 |