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2-Aminobenzaldehyde → 2-(2,6-dichloro-3-nitro-phenyl)-N-(2-formyl-phenyl)-acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Aminobenzaldehyde | HCID 68255 | — |
| 反応物 | 2,6-Dichloro-3-nitrophenylacetic acid | HCID 54265437 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Thionyl Chloride | HCID 24386 | — |
| 生成物 | 2-(2,6-dichloro-3-nitro-phenyl)-N-(2-formyl-phenyl)-acetamide | HCID 59833882 | 88.6% |
反応手順
A solution of (2,6-dichloro-3-nitro-phenyl)-acetic acid (0.90 g, 3.35 mmol) in thionyl chloride (15 mL) is refluxed for one hour. The solvent is removed by concentration and dry toluene is added to thoroughly remove thionyl chloride. To the solution of acid chloride in dry dichloromethane (30 mL) is added (drop-wise) a solution of 2-aminobenzaldehyde (0.365 g, 3.02 mmol) in dichloromethane (5.0 mL). The mixture is stirred at room temperature for 2 hours. The reaction mixture is diluted with EtOAc and washed with saturated K2CO3 and brine. The organic layer is dried, filtered and concentrated to give crude product (0.94 g, 88.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07449582B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-85921cc9266e4e75939cb8df0dbc30ea |
| 出典メモ | uspto-grants-2008_11 |