関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-(4-Chlorophenoxy)aniline | HCID 7578 | — |
| 反応物 | Diphosgene | HCID 10426 | — |
| 反応物 | 3-(4-Chlorophenyl)-4-phenylpyrazoline | HCID 70409590 | — |
| 触媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 70408543 | HCID 70408543 | 53.9% |
反応手順
To a stirred solution of 0.75 g (0.0034 mole) 4-(4-chlorophenoxy)aniline in 25 mL of toluene was added dropwise a solution of 0.43 mL (0.0036 mole) trichloromethylchloroformate in 20 mL of toluene. After complete addition, the mixture was heated at 85° C. for three hours. This mixture was cooled to room temperature and the solvent evaporated under reduced pressure to leave a residue. The residue was dissolved in 25 mL of diethyl ether. This solution was added dropwise to a stirred slurry of 1.0 g (0.0034 mole) of 3-(4-chlorophenyl)-4-phenylpyrazoline in diethyl ether. Three drops of triethylamine were added and the mixture was stirred at room temperature for two days. The solvent was evaporated from the mixture to yield 0.92 g of 3-(4-chlorophenyl)-N-[4-(4-chlorophenoxy)phenyl]-4-phenylpyrazoline-1-carboxamide (mp 158°-161° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04767779 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-0c0d0a5e79614c0a9f11be0474df246f |
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| 出典メモ | uspto-grants-1988_08 |
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