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Triethylamine → 3-Chloro-4-({[3-chloro-4-(trifluoromethyl)benzyl]amino}carbonyl)benzenesulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Chloro-4-(chlorosulfonyl)benzoyl chloride | HCID 19814731 | — |
| 反応物 | 3-Chloro-4-(trifluoromethyl)benzylamine | HCID 23512744 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Chloro-4-({[3-chloro-4-(trifluoromethyl)benzyl]amino}carbonyl)benzenesulfonyl chloride | HCID 57732116 | 40.7% |
反応手順
To a solution of 2-chloro-4-(chlorosulfonyl)benzoyl chloride (J. Org. Chem., 56,16, 1991, 4974) (300 mg, 0.877 mmol, 1 eq) in DCM (3 ml) was added 3-chloro-4-(trifluoromethyl)benzylamine (175 mg, 0.835 mmol, 0.95 eq) and Et3N (33 mg, 0.32 mmol, 0.37 eq) and the reaction mixture stirred at room temperature for 1 hour. The reaction mixture was diluted with ethyl acetate (10 ml), washed with water (10 ml), dried over sodium sulphate, filtered and evaporated. The crude material was purified by column chromatography eluting with ethyl acetate to yield the title compound (154 mg, 0.34 mmol, 39%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08741934B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-d756446f2c68467997e93dcdcb194469 |
| 出典メモ | uspto-grants-2014_06 |