4-(4-Chlorophenoxy)aniline → HCID 70408543, 화합물

HRID 35689

반응식

HRID 35689 반응식
[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

참가 물질

7

반응물 3

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

생성물 1

HCID 70408543HCID 70408543, 화합물수율 53.9%

시약·촉매·용매 3

HCID 8471Triethylamine촉매HCID 1140Toluene용매2회HCID 3283Diethyl Ether용매2회

반응 조건

온도
85 °C

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-0c0d0a5e79614c0a9f11be0474df246f
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04767779

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