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4-Bromo-3-(trifluoromethyl)aniline → 1-(3-Fluoro-5-trifluoromethyl-phenyl)-3-(4-bromo-3-trifluoromethyl-phenyl)-urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Bromo-3-(trifluoromethyl)aniline | HCID 67852 | — |
| 反応物 | 1-Fluoro-3-isocyanato-5-(trifluoromethyl)benzene | HCID 3445672 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(3-Fluoro-5-trifluoromethyl-phenyl)-3-(4-bromo-3-trifluoromethyl-phenyl)-urea | HCID 16755222 | 50% |
反応手順
To a solution of 4-Bromo-3-(trifluoromethyl)-aniline (132 mg, 0.55 mmol, 1.1 eq.) in dry THF (5 ml) was added 3-Fluoro-5-(trifluoromethyl)-phenylisocyanate (72 μl, 0.5 mmol). After stirring overnight at rt the mixture was diluted with cHexane (20 ml), washed twice with 2 N HCl, once with sat. NaHCO3 and brine (20 ml each) and adsorbed on Celite in vacuo. Flash chromatography on silica with cHexane/TBME (4:1 to 2:1) yielded 111 mg product (50%) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07696249B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-29feb1b45952493eafc4fc230a645307 |
| 出典メモ | uspto-grants-2010_04 |