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Acetyl chloride → 2-Ethanoyloxy-5-tert-butoxycarbonylaminobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-(N-tert-Butoxycarbonylamino)salicylic Acid | HCID 10377562 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Ethanoyloxy-5-tert-butoxycarbonylaminobenzoic acid | HCID 22341901 | 52.2% |
反応手順
To a solution of 5-tert-butoxycarbonylamino-2-hydroxybenzoic acid (1.02 g, 4.02 mmole) in DMF (20.0 ml) was added with acetyl chloride (39 mg, 4.83 mmole) and potassium carbonate (555 mg, 4.02 mmole). The reaction mixture was stirred for 4 hr at room temperature. After the reaction mixture was concentrated, the residue was dissolved in ethyl acetate. The organic layer was washed with water and brine and dried over anhydrous Na2SO4. After evaporation of the solvent, the residue was recrystallized from ethyl acetate/hexane to give 0.62 g (52% yield) of 2-ethanoyloxy-5-tert-butoxycarbonylaminobenzoic acid as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07511074B2 |
| 出典データセット | uspto-grants-2009_03 |
| ORD ID | ord-83e2a5dadaef4015baabb40fa38b9712 |
| 出典メモ | uspto-grants-2009_03 |