4-(4-Chlorophenoxy)aniline → HCID 70408543、化合物

HRID 35689

反応式

HRID 35689 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([O:6][C:7]2[CH:13]=[CH:12][C:10]([NH2:11])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.Cl[C:17]([O:20]C(Cl)=O)(Cl)Cl.[Cl:24][C:25]1[CH:30]=[CH:29][C:28]([C:31]2[NH:32][NH:33][CH2:34][C:35]=2[C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[CH:27][CH:26]=1>C1(C)C=CC=CC=1.C(OCC)C.C(N(CC)CC)C>[Cl:24][C:25]1[CH:26]=[CH:27][C:28]([C:31]2[NH:32][N:33]([C:17]([NH:11][C:10]3[CH:12]=[CH:13][C:7]([O:6][C:5]4[CH:14]=[CH:15][C:2]([Cl:1])=[CH:3][CH:4]=4)=[CH:8][CH:9]=3)=[O:20])[CH2:34][C:35]=2[C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)=[CH:29][CH:30]=1

参加物

7

反応物 3

HCID 75784-(4-Chlorophenoxy)anilineHCID 10426DiphosgeneHCID 704095903-(4-Chlorophenyl)-4-phenylpyrazoline

生成物 1

HCID 70408543HCID 70408543、化合物収率 53.9%

試薬・触媒・溶媒 3

HCID 8471Triethylamine触媒HCID 1140Toluene溶媒2 回HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
85 °C

実験手順

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.).

後処理

  1. additionAfter complete addition
  2. temperatureThis mixture was cooled to room temperature
  3. customthe solvent evaporated under reduced pressure
  4. customto leave a residue
  5. customThe solvent was evaporated from the mixture

出典と根拠

ORDレコード
ord-0c0d0a5e79614c0a9f11be0474df246f
出典データセット
uspto-grants-1988_08
特許番号
US04767779

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