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Acetic Anhydride → N-acetyl-5-bromo-3-formyl-4-methoxybenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Bromo-5-formyl-4-methoxy-benzenesulfonamide | HCID 86607698 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-acetyl-5-bromo-3-formyl-4-methoxybenzenesulfonamide | HCID 86607697 | 91.6% |
反応手順
A 100 mL round-bottom flask was charged with 5-bromo-3-formyl-4-methoxy-benzenesulfonamide (586 mg, 2.0 mmol) dissolved in dichloromethane (40 mL) and the solution was stirred vigorously while triethylamine (252 mg, 2.50 mmol) was added, followed by acetic anhydride (224 mg, 2.2 mmol) and a catalytic amount of N,N-dimethylaminopyridine. The mixture was stirred for 1 hour and then concentrated by evaporation. The residue was partitioned between 5% citric acid and ethyl acetate. The organic layer was separated, washed with water and brine and dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to give N-acetyl-5-bromo-3-formyl-4-methoxybenzenesulfonamide (616 mg) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09162986B2 |
| 出典データセット | uspto-grants-2015_10 |
| ORD ID | ord-96a38c5c9e364032a7fe4b8960f139ae |
| 出典メモ | uspto-grants-2015_10 |