Dichloroacetyl chloride → 5-Dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole

HRID 34859

반응식

HRID 34859 반응식
C(=O)([O-])[O-].[Na+].[Na+].[Cl:7][CH:8]([Cl:12])[C:9](Cl)=[O:10].[NH2:13][C:14]1[N:18]([C:19]2[C:24]([Cl:25])=[CH:23][C:22]([C:26]([F:29])([F:28])[F:27])=[C:21]([Cl:30])[C:20]=2[Cl:31])[N:17]=[CH:16][CH:15]=1>ClCCl>[Cl:7][CH:8]([Cl:12])[C:9]([NH:13][C:14]1[N:18]([C:19]2[C:24]([Cl:25])=[CH:23][C:22]([C:26]([F:29])([F:27])[F:28])=[C:21]([Cl:30])[C:20]=2[Cl:31])[N:17]=[CH:16][CH:15]=1)=[O:10]

참가 물질

5

반응물 3

HCID 6593Dichloroacetyl chlorideHCID 10340Sodium CarbonateHCID 136896131H-Pyrazol-5-amine, 1-[2,3,6-trichloro-4-(trifluoromethyl)phenyl]-

생성물 1

HCID 139134305-Dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole수율 93.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

15.3 g (0.145 mol) of anhydrous sodium carbonate and 4.76 ml (0.048 mol) of 98% strength dichloroacetyl chloride are added in succession, at 5° C. to 10° C., to 8.0 g (0.024 mol) of 5-amino-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole in 80 ml of dichloromethane. The mixture is stirred for 4 hours at 5° C.-10° C. and for 13 hours at room temperature. The mixture is diluted with 80 ml of dichloromethane, filtered, and washed in succession with water and saturated sodium chloride solution. The organic phase is dried over magnesium sulphate and freed from the solvent in vacuo. 10.0 g (93.5% of theory) of 5-dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole of melting point 156° C.-161° C. are obtained.

후처리

  1. filtrationfiltered
  2. washwashed in succession with water and saturated sodium chloride solution
  3. dry with materialThe organic phase is dried over magnesium sulphate

출처 및 근거

ORD 기록
ord-c3d814524d1c47dabe278a17cca85bd0
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764202

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