化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → [2-[[3,5-bis(trifluoromethyl)phenyl]carbamoyl]-4-chloro-phenyl] Acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Imd-0354 | HCID 5081913 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [2-[[3,5-bis(trifluoromethyl)phenyl]carbamoyl]-4-chloro-phenyl] Acetate | HCID 9979865 | 83% |
反応手順
N-[3,5-Bis(trifluoromethyl)phenyl]-5-chloro-2-hydroxybenzamide (1.51 g, 3 mmol) and pyridine (285 mg, 3.6 mmol) were dissolved in tetrahydrofuran (6 mL). Acetyl chloride (234 mg, 3.3 mmol) was added dropwise under ice cooling, and the mixture was stirred at room temperature for 1 hour. The solvent was evaporated under reduced pressure. 2 N hydrochloric acid was added to the residue, and it was extracted with ethyl acetate. After the ethyl acetate layer was washed with water and brine, dried over anhydrous magnesium sulfate and concentrated, the residue was recrystallized from n-hexane-ethyl acetate to give the title compound (1.06 g, 83.0%) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08097759B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-601c0910dbb74169b4d5c7462ea9c473 |
| 出典メモ | uspto-grants-2012_01 |