関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-Chloro-2-nitroaniline | HCID 6979 | — |
| 反応物 | Benzenesulfonyl chloride | HCID 7369 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(4-Chloro-2-nitrophenyl)benzenesulfonamide | HCID 555628 | — |
反応手順
To a solution of 2-nitro-4-chloroaniline (500 mg) and pyridine (2.1 ml in methylene chloride (10 ml), benzenesulfonylchloride (1.2 ml) was added dropwise at 0° C. under an atmosphere of argon. The reaction mixture was stirred for 3 days at room temperature. To the reaction mixture, water was added. The mixture was extracted with ethyl acetate. The organic layer was washed, dried over and concentrated under the reduced pressure. The reside was recrystallized from AcOEt-hexane mixture solvent to give the by-product. The mother liquor was concentrated under the reduced pressure. The residue was purified on silica gel column chromatography (AcOEt-hexane) and recrystallized from AcOEt-hexane mixture solvent to give the title compound (175 mg) having the following physical data.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06448290B1 |
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| 出典データセット | uspto-grants-2002_09 |
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| ORD ID | ord-233de6277ac44ef7b0f02fea12d39e9c |
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| 出典メモ | uspto-grants-2002_09 |
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