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Benzenesulfonamide → N-benzenesulfonyl-4-acetylamino-3-nitrobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzenesulfonamide | HCID 7370 | — |
| 反応物 | 4-Acetamido-3-nitrobenzoic acid | HCID 73758 | — |
| 反応物 | 3-(Cycloundecen-1-yl)-1,2-diazacycloundec-2-ene | HCID 53630274 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-benzenesulfonyl-4-acetylamino-3-nitrobenzamide | HCID 18315416 | 78.2% |
反応手順
N,N′-carbonyldiimidazole (14.45 g) was added to a solution of 10.00 g of 4-acetylamino-3-nitrobenzoic acid in 300 ml of N,N-dimethylformamide, and the mixture was stirred at room temperature for 1 hour. Subsequently, 14.03 g of benzenesulfonamide and 13.58 g of diazabicycloundecene were added thereto, and the mixture was stirred at 100° C. for 72 hours. The reaction mixture was separated with the addition of chloroform and water. The organic layer was then concentrated, and the resulting residue was purified through silica-gel column chromatography (eluent: a mixture of ethyl acetate and methanol at a ratio of 4:1) to give 12.67 g of N-benzenesulfonyl-4-acetylamino-3-nitrobenzamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06352985B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-5431c869c2e0400b9d0d9f80ddb4dede |
| 出典メモ | uspto-grants-2002_03 |