化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → N-(3-Cyano-4-isobutylphenyl)-1-(4-fluorophenyl)-3-methylpyrazole-4-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Diethyl cyanophosphonate | HCID 76257 | — |
| 反応物 | 5-Amino-2-(2-methylpropyl)benzonitrile | HCID 22227932 | — |
| 反応物 | 1-(4-fluorophenyl)-3-methyl-1H-pyrazole-4-carboxylic acid | HCID 22228057 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(3-Cyano-4-isobutylphenyl)-1-(4-fluorophenyl)-3-methylpyrazole-4-carboxamide | HCID 22228075 | 35.1% |
反応手順
1-(4-Fluorophenyl)-3-methylpyrazole-4-carboxylic acid (1.5 g), 5-amino-2-isobutylbenzonitrile (1.2 g), triethylamine (2.0 g) and diethyl cyanophosphate (1.2 g) were added to dimethylformamide (15 ml) and the mixture was stirred at room temperature for 1 h. The reaction mixture was added into water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. A mixed solvent of ethyl acetate-n-hexane was added to the residue to allow crystallization. The crystals were recrystallized from hydrous dimethylformamide to give the title compound (0.9 g), melting point: 178–179° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07015218B1 |
| 出典データセット | uspto-grants-2006_03 |
| ORD ID | ord-29466eef691b4b4a9665ab182fc32d67 |
| 出典メモ | uspto-grants-2006_03 |