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Triethylamine → 1-(o-tolyl)-3-(3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propyl)urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Tolyl isocyanate | HCID 69194 | — |
| 反応物 | 3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propan-1-amine | HCID 90404268 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(o-tolyl)-3-(3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propyl)urea | HCID 118675079 | 53% |
反応手順
In a 25 mL flask, to a solution of 3-(4-(1-(4-(trifluoromethoxy)phenyl)-1H-1,2,4-triazol-3-yl)phenyl)propan-1-amine (0.160 g, 0.442 mmol) in dichloromethane (2 mL) was added 2-methyl phenylisocyanate (0.06 g, 0.497 mmol) in dichloromethane (5 mL) followed by triethylamine (0.044 g, 0.414 mmol). The reaction mixture was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate and adsorbed onto Celite®. Purification by flash column chromatography (reverse phase) 5% acetonitrile/water provided the title compound as a white solid (0.11 g, 53%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09445594B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-7fed12727651473aadfe67fb4bbfbc95 |
| 出典メモ | uspto-grants-2016_09 |