化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → 2-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]benzoic Acid Methyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-Fluoro-2-(trifluoromethyl)aniline | HCID 67853 | — |
| 反応物 | Benzoic acid, 2-(chlorosulfonyl)-, methyl ester | HCID 117830 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]benzoic Acid Methyl Ester | HCID 53972694 | — |
反応手順
250 ml of dichloromethane is combined with 9.38 g (52.37 mmol) of 4-fluoro-2-trifluoromethylaniline and 6 ml (14.3 mmol) of pyridine. The mixture is cooled with ice water and under agitation and exclusion of moisture, 13.52 g (57.62 mmol) of 2-chlorosulfonylbenzoic acid methyl ester is added in small increments. The mixture is agitated overnight, washed with 2N hydrochloric acid and water, the dichloromethane solution is dried over sodium sulfate and concentrated to dryness under vacuum. The residue is crystallized from ethyl acetate/hexane. The title compound melts at 143°-145° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05210290 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-a6fedd8e9f7a413da2a41d0ee8a8f102 |
| 出典メモ | uspto-grants-1993_05 |