関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | o-Toluenesulfonyl chloride, 5-nitro- | HCID 8457 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-Methyl-5-nitrobenzene-1-sulfonamide | HCID 234282 | 38% |
反応手順
In a round bottom flask under nitrogen was placed commercially available 2-methyl-5-nitrobenzene sulphonyl chloride (2.36 g, 10.0 mmol) and 75 L dry ethyl ether was added. The solution was cooled to 0° C. and concentrated ammonium hydroxide (10 mL) was added. After stirring overnight, the mixture was filtered and then diluted with dichloromethane (150 mL). The organic layer was separated and dried over MgSO4. The solution was then concentrated to afford 820 mg of the title compound as a white solid (38%): 1HNMR (DMSO-d6) δ8.61 (d, J=2.5 Hz, 1H), 8.35 (dd, J=8 Hz, 2.5 Hz, 1H), 7.79 (br s, 2H), 7.70 (d, J=8 Hz, 1H), 2.71 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06355633B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-67f09f193ae047fe86dd166c0ea4709f |
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| 出典メモ | uspto-grants-2002_03 |
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