関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfamic Acid | HCID 5987 | — |
| 反応物 | 2-Nitrotoluene | HCID 6944 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 生成物 | 4-Methyl-3-nitrobenzenesulfonyl chloride | HCID 560638 | — |
反応手順
137.1 g (1.0 mol) of o-nitrotoluene are added dropwise to 535.9 g (4.6 mol) of chlorosulfonic acid and 2 g of sulfamic acid such that the temperature does not exceed 40° C. The mixture is then stirred at 40° C. for 1 hour and slowly heated to 105° C. It is then stirred at 105° C. for 6 hours, cooled and added dropwise to ice water at 0 to 5° C. The precipitated crystals are filtered off with suction and washed with ice water. 236.1 g of 2-nitrotoluene-4-sulfonyl chloride (water content 10.8%), corresponding to 210.6 g (89% of theory), having a melting point of 40° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05136043 |
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| 出典データセット | uspto-grants-1992_08 |
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| ORD ID | ord-8a977c20515740ad9993a4aecce97da6 |
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| 出典メモ | uspto-grants-1992_08 |
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