Ammonium Hydroxide → 1-(2,4-Dichlorophenyl)-5-(trifluoromethyl)-1h-pyrazole-4-carboxamide

HRID 1284403노트

반응식

HRID 1284403 반응식
[F:1][C:2]([F:20])([F:19])[C:3]1[N:7]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=2[Cl:15])[N:6]=[CH:5][C:4]=1[C:16](O)=[O:17].C(N1C=CN=C1)([N:23]1C=CN=C1)=O.[OH-].[NH4+]>CN(C=O)C>[F:1][C:2]([F:20])([F:19])[C:3]1[N:7]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=2[Cl:15])[N:6]=[CH:5][C:4]=1[C:16]([NH2:23])=[O:17]

참가 물질

5

반응물 3

HCID 14923Ammonium HydroxideHCID 682631,1'-CarbonyldiimidazoleHCID 13537979HCID 13537979, 화합물

생성물 1

HCID 1904701-(2,4-Dichlorophenyl)-5-(trifluoromethyl)-1h-pyrazole-4-carboxamide수율 61.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

5-(Trifluoromethyl)-1-(2,4-dichlorophenyl)-1H-pyrazole-4-carboxylic acid (5.0 grams, 0.015 mole) and carbonyldiimidazole (2.74 grams, 0.017 mole) were dissolved in 35 ml of DMF. The solution was stirred for 10 minutes and ammonium hydroxide (8 ml) was then added. The reaction mixture was stirred at room temperature for 72 hours, then poured into 150 ml of ice/water. The product precipitated and was separated by filtration, dried, and recrystallized from toluene with charcoal, yielding 3.0 grams of 5-(trifluoromethyl)-1-(2,4-dichlorophenyl)-1H-pyrazole-4-carboxamide, mp=191°-193° C.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 72 hours
  2. customThe product precipitated
  3. customwas separated by filtration
  4. customdried
  5. customrecrystallized from toluene with charcoal

출처 및 근거

ORD 기록
ord-8e6f77f6c2fe4195b7ee7178a3de2dbb
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04563210

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