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P-Phenylenediamine → N-(4-chloro-3-(trifluoromethyl)phenyl)-N'-(4-aminophenyl)urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | P-Phenylenediamine | HCID 7814 | — |
| 反応物 | 1-Chloro-4-isocyanato-2-(trifluoromethyl) benzene | HCID 2733265 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(4-chloro-3-(trifluoromethyl)phenyl)-N'-(4-aminophenyl)urea | HCID 23614594 | 97.2% |
反応手順
To a solution of 4-chloro-3-(trifluoromethyl)phenyl isocyanate (2.27 g, 10.3 mmol) in CH2Cl2 (308 mL) was added p-phenylenediamine (3.32 g, 30.7 mmol) in one part. The resulting mixture was stirred at room temp. for 1 h, treated with CH2Cl2 (100 mL), and concentrated under reduced pressure. The resulting pink solids were dissolved in a mixture of EtOAc (110 mL) and MeOH (15 mL), and the clear solution was washed with a 0.05 N HCl solution. The organic layer was concentrated under reduced pressure to afford impure N-(4-chloro-3-(trifluoromethyl)phenyl)-N′-(4-aminophenyl)urea (3.3 g): TLC (100% EtOAc) Rf 0.72.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841330B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-1d4590b940d34104bce128bf5fcbbd34 |
| 出典メモ | uspto-grants-2014_09 |