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1H-1,2,4-Triazole → HCID 12765983, 화합물

HRID 1995925
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HRID 1995925 반응식
BrBr.[Cl:3][C:4]1[CH:25]=[CH:24][C:7]([O:8][CH2:9][C:10](=[O:23])[C:11]([CH3:22])([CH3:21])[CH2:12][S:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[CH:6][CH:5]=1.[NH:26]1[CH:30]=[N:29][CH:28]=[N:27]1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)(Cl)Cl>[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([O:8][CH:9]([N:26]2[CH:30]=[N:29][CH:28]=[N:27]2)[C:10](=[O:23])[C:11]([CH3:21])([CH3:22])[CH2:12][S:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[CH:24][CH:25]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 24408BromineHCID 127659751-(4-Chlorophenoxy)-4-(4-chlorophenylmercapto)-3,3-dimethyl-butan-2-one

생성물 1

HCID 12765983HCID 12765983, 화합물수율 26%

시약·촉매·용매 1

HCID 5943
Carbon Tetrachloride
용매

실험 절차

48 g (0.3 mol) of bromine were added dropwise to 110.5 g (0.3 mol) of 1-(4-chlorophenoxy)-4-(4-chlorophenylmercapto)-3,3-dimethyl-butan-2-one in 750 ml of carbon tetrachloride at room temperature. The mixture was subsequently stirred at room temperature for one hour and was concentrated by distilling off the solvent in vacuo, and the residue was taken up in 750 ml of toluene. 73 g (1.06 mol) of 1,2,4-triazole and 150 g (1.06 mol) of potassium carbonate were added to this solution. The mixture was heated to 90° C. for 8 hours and allowed to cool to room temperature and the organic phase was separated off. This phase was extracted with dilute sodium hydroxide solution, rinsed with water, dried over sodium sulphate and concentrated in vacuo. 34 g (26% of theory) of 1-(4-chlorophenoxy)-4-(4-chlorophenylmercapto)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one of melting point 115° C. were obtained.

후처리

  1. concentrationwas concentrated
  2. distillationby distilling off the solvent in vacuo
  3. temperatureThe mixture was heated to 90° C. for 8 hours
  4. temperatureto cool to room temperature
  5. customthe organic phase was separated off
  6. extractionThis phase was extracted with dilute sodium hydroxide solution
  7. washrinsed with water
  8. dry with materialdried over sodium sulphate
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b03004be0eab43d6b40fb7c566bc40e4
출처 데이터셋
uspto-grants-1983_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04406909

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