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Methanol → 2-[2-(2,4,5-Trichloro-phenoxy)-acetylamino]-isonicotinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Trichlorophenoxyacetic acid | HCID 1480 | — |
| 反応物 | 2-Aminoisonicotinamide | HCID 351653 | — |
| 反応物 | PyBOP | HCID 2724699 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[2-(2,4,5-Trichloro-phenoxy)-acetylamino]-isonicotinamide | HCID 58001320 | 41.1% |
反応手順
To solution of (2,4,5-trichloro-phenoxyacetic acid (100 mg, 0.39 mmol), 2-amino isonicotinamide (107 mg, 0.78 mmol) and DMAP (96.22 mg, 0.78 mmol) in DMF 12 ml was added PyBOP (409.7 mg, 0.78 mmol), and stirred room temperature. Reaction mixture was poured onto ice cold water, diluted by methanol/MC mixture (10%). The organic phase was separated, sequentially washed with aqueous sodium bicarbonate, brine and water, dried over anhydrous MgSO4, and concentrated. The residue was purified by PLC (EtoAC:Hexane:MeOH=3:6:1-2:4:1) to afford 2-[2-(2,4,5-trichloro-phenoxy)-acetylamino]-isonicotinamide as a colorless solid (0.06 g, 41% 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-474952af8a0f467a9705947702d17dea |
| 出典メモ | uspto-grants-2013_03 |