化工社化工社 化学情報印刷レポート · 研究参考用
Toluene → Imd-0354
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 5-Chlorosalicylic Acid | HCID 9447 | — |
| 反応物 | Benzenamine, 3,5-bis(trifluoromethyl)- | HCID 9480 | — |
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Imd-0354 | HCID 5081913 | 85.5% |
反応手順
A mixture of 5-chlorosalicylic acid(6.90 g, 40 mmol), 3,5-bis(trifluoromethyl)aniline(9.16 g, 40 mmol), phosphorus trichloride(1.74 mL, 20 mmol) and toluene(80 mL) was refluxed for 3 hours under argon atmosphere. After the reaction mixture was cooled to room temperature, it was diluted with ethyl acetate (240 mL). After the ethyl acetate layer was washed successively with water and brine, dried over anhydrous magnesium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=4:1) to give the title compound (13.12 g, 85.5%) as a light yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07626042B2 |
| 出典データセット | uspto-grants-2009_12 |
| ORD ID | ord-15e5a58d6dda499799ed9adf297e061d |
| 出典メモ | uspto-grants-2009_12 |