Pyridine → 5-(2,4-Dichlorophenoxyacetamido)-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole

HRID 569709노트

반응식

HRID 569709 반응식
N1C=CC=CC=1.[Cl:7][C:8]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:9]=1[O:10][CH2:11][C:12](Cl)=[O:13].[NH2:20][C:21]1[N:25]([C:26]2[C:31]([Cl:32])=[CH:30][C:29]([C:33]([F:36])([F:35])[F:34])=[CH:28][C:27]=2[Cl:37])[N:24]=[CH:23][CH:22]=1>ClCCl>[Cl:7][C:8]1[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:9]=1[O:10][CH2:11][C:12]([NH:20][C:21]1[N:25]([C:26]2[C:31]([Cl:32])=[CH:30][C:29]([C:33]([F:34])([F:36])[F:35])=[CH:28][C:27]=2[Cl:37])[N:24]=[CH:23][CH:22]=1)=[O:13]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 69887(2,4-Dichlorophenoxy)acetyl chlorideHCID 135571095-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole

생성물 1

HCID 139117395-(2,4-Dichlorophenoxyacetamido)-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole수율 94.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

2.2 ml (0.0275 mol) of anhydrous pyridine and 6.7 g (0.027 mol) of 96.3 percent strength 2,4-dichlorophenoxyacetyl chloride are added successively to 8 g (0.027 mol) of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole (cf. U.S. Pat. No. 4,614,533, supra, in 60 ml of dichloromethane with stirring at 0° C. to 5° C. and the mixture is stirred for 16 hours at room temperature. The mixture is worked up by adding 100 ml of dichloromethane, washing successively with dilute hydrochloric acid, saturated sodium bicarbonate solution and saturated sodium chloride solution, drying the organic phase over magnesium sulphate and removing the solvent in vacuo. 12.7 g (94.3% of theory) of 5-(2,4-dichlorophenoxyacetamido)-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole of melting point 167° C.-180° C. are obtained.

후처리

  1. washwashing successively with dilute hydrochloric acid, saturated sodium bicarbonate solution and saturated sodium chloride solution
  2. dry with materialdrying the organic phase over magnesium sulphate
  3. customremoving the solvent in vacuo

출처 및 근거

ORD 기록
ord-55b6c277f7e24b56919f2ba491507085
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04734125

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