関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzenesulfonamide | HCID 7370 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 2-[4-(2-Butylbenzimidazol-1-yl)methylphenyl]benzoic acid | HCID 4110026 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium chloride ethyl acetate | HCID 86643102 | — |
| 生成物 | HCID 15104381 | HCID 15104381 | — |
反応手順
960 mg (2.5 mmol) of 4'-[(2-n-butyl-benzimidazol-1-yl)-methyl]biphenyl-2-carboxylic acid are dissolved in 25 ml of methylene chloride, treated with 2 ml of thionyl chloride and heated under reflux for one hour. The solvent is then distilled off and evaporated 2 times after adding methylene chloride. 390 mg (2.5 mmol) of benzenesulphonamide are added to the residue and the mixture is heated for one hour at 140° C. After cooling, the oil obtained is taken up in ethyl acetate/sodium chloride solution and extracted 3 times using ethyl acetate. The combined ethyl acetate phases are dried over sodium sulphate, evaporated and the crude product obtained is purified over a silica gel column using methylene chloride/ethanol as eluting agent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05864043 |
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| 出典データセット | uspto-grants-1999_01 |
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| ORD ID | ord-62db22f44978472f964c5b6bd9136ec7 |
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| 出典メモ | uspto-grants-1999_01 |
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