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4-Toluenesulfonyl chloride → (Tetrahydrofuran-2,5-diyl)bis(methylene) bis(4-methylbenzenesulfonate)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | 2,5-Tetrahydrofurandimethanol | HCID 97792 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (Tetrahydrofuran-2,5-diyl)bis(methylene) bis(4-methylbenzenesulfonate) | HCID 259634 | — |
反応手順
34.0 g (261 mmol) of 2,5-bis(hydroxymethyl)tetrahydrofuran are dissolved in 260 ml of dichloromethane. A solution of 99.0 g (521 mmol) of p-toluenesulfonyl chloride in 52 ml of pyridine and 130 ml of dichloromethane is added dropwise thereto. After stirring at room temperature for 24 hours, the precipitate is filtered off with suction and washed with dichloromethane. The filtrate and the washing phases are combined, washed with dilute hydrochloric acid and then with saturated aqueous sodium bicarbonate solution, dried over magnesium sulfate and evaporated to dryness. The crude product is recrystallized from ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091198B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-2b5e20797f2d4f3f95674291e28ba251 |
| 出典メモ | uspto-grants-2006_08 |