関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Methyl-4-nitroaniline | HCID 7441 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 触媒 | Copper Sulfate | HCID 24462 | — |
| 生成物 | 5-Nitrotoluene-2-sulfonyl chloride | HCID 88869 | 85% |
反応手順
200 Parts by weight of 1-amino-2-methyl-4-nitrobenzene were diazotized at 0° - 5° C with 400 parts by weight of 30% hydrochloric acid and 235 parts by weight of 40% sodium nitrite solution. The clarified diazo solution was allowed to run, with slight external cooling, below the surface of a mixture of 1300 parts by weight of 30% hydrochloric acid, 33 parts by weight of crystalline copper sulfate and 330 parts by weight of 40% sodium bisulfite lye, while adding at the same time further 330 parts by weight of 40% sodium bisulfite lye. After about 45 minutes, the sulfonic acid chloride that had separated was filtered off with suction, washed with 2000 parts by volume of cold water and dried. The 2-methyl-4-nitrobenzene-sulfonic acid chloride was obtained in a yield of 85% of the theory and was found to melt at 105° - 106° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03947512 |
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| 出典データセット | uspto-grants-1976_03 |
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| ORD ID | ord-07874c6319e44858a530e7aaa4a60651 |
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| 出典メモ | uspto-grants-1976_03 |
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