関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 4-Cyclohexylbenzenesulfonic Acid Sodium Salt | HCID 23694893 | — |
| 生成物 | 4-Cyclohexylbenzene-1-sulfonyl chloride | HCID 4339442 | — |
反応手順
The sodium salt prepared in Example I (420 gm, 1.6M) is intermittently mixed with phosphorous pentachloride (160 gm, 0.77M) in a three liter multi-necked flask and slowly warmed to 70° C. in an oil bath. The liquified reaction mass is aged at 70° C. for 8 hours, then cooled to room temperature and carefully poured over one kilogram of cracked ice. A solid precipitate is removed by filtration and the aqueous phase is extracted with methylene chloride three times, each time using 300 milliliters of MeCl. The combined organic phases are dried and concentrated using a rotary evaporator. 4-cyclohexylbenzenesulfonyl chloride (338 gm, 81% of theoretical yield) was recovered as a crude product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04764239 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-3edceb04c1ea4df588859da19aabf28a |
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| 出典メモ | uspto-grants-1988_08 |
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