Water → 5-(2-chloro-6-fluorophenyl)-3-(4-chloro-alpha,alpha-dimethylbenzyl)-1-methyl-1H-1,2,4-triazole

HRID 443045

반응식

HRID 443045 반응식
[CH3:1][C:2]([C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)([CH3:7])[C:3](Cl)=[N:4][NH2:5].[Cl:15][C:16]1[CH:23]=[CH:22][CH:21]=[C:20]([F:24])[C:17]=1[C:18]#[N:19].[Cl-].[Al+3].[Cl-].[Cl-].O.Cl[C:31]1C=CC=CC=1Cl>>[Cl:15][C:16]1[CH:23]=[CH:22][CH:21]=[C:20]([F:24])[C:17]=1[C:18]1[N:5]([CH3:31])[N:4]=[C:3]([C:2]([CH3:7])([CH3:1])[C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[N:19]=1

참가 물질

6

반응물 5

HCID 962WaterHCID 72391,2-DichlorobenzeneHCID 695872-Chloro-6-fluorobenzonitrileHCID 6451240Aluminum(III) ChlorideHCID 86754043alpha, alpha-Dimethyl-4-chlorophenylacetohydrazonoyl chloride

생성물 1

HCID 542307375-(2-chloro-6-fluorophenyl)-3-(4-chloro-alpha,alpha-dimethylbenzyl)-1-methyl-1H-1,2,4-triazole

반응 조건

온도
120 °C

실험 절차

To a solution of 0.7 g of N-methyl-N-(p-toluenesulfonyl)-(α, α-dimethyl-4-chlorophenylacetohydrazonoyl chloride in 7 ml of o-dichlorobenzene at room temperature, were added 0.33 g of 2-chloro-6-fluorobenzonitrile and 0.28 g of anhydrous aluminium chloride, and the reaction mixture was heated at 120° C. for 30 minutes. After cooling, the reaction mixture was poured into iced water and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to afford 0.6 g of 5-(2-chloro-6-fluorophenyl)-3-(4-chloro-α,α-dimethylbenzyl)-1-methyl-1H-1,2,4-triazole. m.p.97°-100° C.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d78e0ccdc1964e0599130b92559e95f0
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05892048

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