関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Sulfolane | HCID 31347 | — |
| 反応物 | Benzenesulfonic acid, 2-chloro-5-nitro-, sodium salt (1:1) | HCID 70350 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Chloro-5-nitrobenzenesulfonyl chloride | HCID 20630 | — |
反応手順
To a mixture of 104 g of commercially available sodium 2-chloro-5-nitrobenzenesulfonate, 200 ml of acetonitrile and 200 ml of sulfolane stirred at 25° C., was added 153 ml of phosphorus oxychloride over a period of 30 minutes. The temperature was not allowed to exceed 40° C. After completion of the addition, the reaction mixture was heated to 70° C. for 1.5 hours. On cooling to 0° C., the reaction mixture was poured over ice. The resulting solid product was washed with cold water, filtered and air-dried to give 77.6 g of the title compound with a melting point of 87°-89° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05324854 |
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| 出典データセット | uspto-grants-1994_06 |
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| ORD ID | ord-c43d1870def748829329065843f91042 |
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| 出典メモ | uspto-grants-1994_06 |
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