化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → N-Des(isobutyraldehyde) Pyflubumide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | trimethyl-1H-pyrazole-4-carbonyl chloride | HCID 13637622 | — |
| 反応物 | 3-Isobutyl-4-[1-methoxy-2,2,2-trifluoro-1-(trifluoromethyl)ethyl]aniline | HCID 86619003 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-Des(isobutyraldehyde) Pyflubumide | HCID 86629858 | 80% |
反応手順
1,3,5-trimethylpyrazole-4-carbonyl chloride (3.93 g, 22.8 mmol), 3-isobutyl-4-[1-methoxy-2,2,2-trifluoro-1-(trifluoromethyl)ethyl]aniline (5.0 g, 15.2 mmol), and triethylamine (3.07 g, 30.4 mmol) were dissolved in tetrahydrofuran (100 ml), and the mixture was heated under reflux for 5 hr. The reaction mixture was diluted with ethyl acetate, and washed with water. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained crude crystals were washed with ether to give the desired compound (5.62 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08404861B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-fc21d52197af4bf697b743186097cfcb |
| 出典メモ | uspto-grants-2013_03 |