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1,2-Dichloroethane → 3-[2-(2,4,5-Trichloro-phenoxy)acetyl-amino]-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Trichlorophenoxyacetic acid | HCID 1480 | — |
| 反応物 | 3-Aminobenzamide | HCID 1645 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-[2-(2,4,5-Trichloro-phenoxy)acetyl-amino]-benzamide | HCID 24811105 | 84.9% |
反応手順
To a solution of the 2,4,5-trichloro-phenoxy acetic acid (76.7 mg, 0.3 mmol), 3-amino benzamide (61.3 mg, 0.45 mmol), EDC (86.3 mg, 0.45 mmol) and HOBt (61.3 mg, 0.45 mmol) were dissolved in DMF (3 mL), and DIPEA (0.08 mL, 0.45 mmol) were added. The reaction mixture was stirred at room temperature overnight, and then partitioned between Ethyl acetate and brine. The organic phase was dried (anhydrous MgSO4), and concentrated. Purification by silica gel column chromatography (CH2Cl2:MeOH=6:3:1) gave 3-[2-(2,4,5-trichloro-phenoxy)acetyl-amino]-benzamide as a white solid (95.2 mg, 84.9% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08394799B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-1638c6b9dae34265b2de453734b00d69 |
| 出典メモ | uspto-grants-2013_03 |