関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Iodobenzenesulfonyl chloride | HCID 7399 | — |
| 反応物 | 2-Amino-5-chlorobenzophenone | HCID 12870 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(2-benzoyl-4-chloro-phenyl)-4-iodo-benzenesulfonamide | HCID 10028837 | — |
反応手順
To a magnetically stirred solution of 2-amino-5-chlorobenzophenone (1.62 g, 7.0 mmol) in dry pyridine (30 mL) was added dropwise a solution of pipsyl chloride in toluene (12 mL) and the reaction was stirred at ambient temperature. The reaction was added to cold (ice bath) 6M hydrochloric acid with stirring and the mixture was extracted with ethyl acetate (3×50 mL). The extracts were washed with water and with saturated aqueous NaCl. The organic layer was dried (MgSO4), filtered and concentrated to give a crystalline solid. The product was filtered, washed with hexane and dried (vacuum) to get white crystalline solid. 1H NMR (CDCl3) δ 9.63 (br s, 1H, NH), 7,75 (dm, 1H, J=8.8 Hz), 7.62 (tm, 1H, J=7.6 Hz), 7.56 (dm, 1H, J=7.6 Hz), 7.48 (m, 3H), 7.32 (m, 5H). MS: m/z 498.0 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741519B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-b0a0b1bcdaaa45ae94632dc13858f9ea |
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| 出典メモ | uspto-grants-2010_06 |
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