関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Dodecylbenzenesulphonic acid | HCID 25457 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Dodecylbenzene-1-sulfonyl chloride | HCID 20439001 | — |
反応手順
To a solution composed of 32.7 g (0.1 mol) of dodecylbenzenesulfonic acid, 80 ml of ethyl acetate, and 12 ml of dimethylformamide (DMF) was added dropwise 12.4 ml (0.15 mol) of phosphorus oxychloride with stirring over a period of 10 minutes and then while heating the mixture so as to maintain the temperature thereof at 40° C., the reaction was performed for 60 minutes. After the reaction was over, the reaction mixture was cooled to 5° to 10° C. and then a solution composed of 16 g of sodium chloride and 160 ml of water was added dropwise to the reaction mixture over a period of 15 minutes. After removing an aqueous layer, an ethyl acetate layer thus formed was washed once with 100 ml of an aqueous 10% sodium chloride solution. The ethyl acetate solution of dodecylbenzenesulfonyl chloride obtained was used for the subsequent reaction as it was.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04547452 |
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| 出典データセット | uspto-grants-1985_10 |
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| ORD ID | ord-3512c7e676b14115b288d83f8d6f60e5 |
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| 出典メモ | uspto-grants-1985_10 |
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