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Potassium Carbonate → 7-Bromo-5-methoxy-N,N-dimethylbenzofuran-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-chloro-N,N-dimethylacetamide | HCID 75886 | — |
| 反応物 | 3-Bromo-2-hydroxy-5-methoxybenzaldehyde | HCID 735818 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-Bromo-5-methoxy-N,N-dimethylbenzofuran-2-carboxamide | HCID 59636744 | — |
反応手順
3-Bromo-2-hydroxy-5-methoxybenzaldehyde (1.5 g, 6.49 mmol), 2-chloro-N,N-dimethylacetamide (0.73 mL, 7.14 mmol) and potassium carbonate (1.8 g, 13.0 mmol) were heated to reflux in dimethylformamide (15 mL) for 2 h. The solvent was removed in vacuo and the residue was taken up in ethyl acetate and washed with water and brine. The organic phase was dried over MgSO4, filtered and then concentrated by rotary evaporation. The crude product was purified by flash chromatography (SiO2; heptane/EtOAc, gradient 0-100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08859534B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-40358d7246024d398159dbea5d096d44 |
| 出典メモ | uspto-grants-2014_10 |