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Water → 1-(2,3,5,6-Tetrafluoro-4-trifluoromethylphenyl)-5-methylcarbonylaminopyrazole

HRID 2232177
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HRID 2232177 반응식
C(O[C:5](=[O:7])[CH3:6])(=O)C.[NH2:8][C:9]1[N:13]([C:14]2[C:19]([F:20])=[C:18]([F:21])[C:17]([C:22]([F:25])([F:24])[F:23])=[C:16]([F:26])[C:15]=2[F:27])[N:12]=[CH:11][CH:10]=1.O>C(O)(=O)C>[C:5]([NH:8][C:9]1[N:13]([C:14]2[C:19]([F:20])=[C:18]([F:21])[C:17]([C:22]([F:25])([F:24])[F:23])=[C:16]([F:26])[C:15]=2[F:27])[N:12]=[CH:11][CH:10]=1)(=[O:7])[CH3:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 7918Acetic AnhydrideHCID 139337095-Amino-1-(2,3,5,6-tetrafluoro-4-trifluoromethylphenyl)pyrazole

생성물 1

HCID 139337111-(2,3,5,6-Tetrafluoro-4-trifluoromethylphenyl)-5-methylcarbonylaminopyrazole수율 87.7%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

250 ml (0.26 mol) of acetic anhydride are added to 60 g (0.20 mol) of 5-amino-1-(2,3,5,6-tetrafluoro-4-trifluoromethyl-phenyl)-pyrazole in 170 ml glacial acetic acid, whereupon the reaction temperature rises from 20° C. to about 35° C. The mixture is stirred at room temperature for 16 hours and then poured onto 800 ml of water. The crystalline solid which has precipitated out is filtered off with suction, washed freely with water and acetic acid and dried in vacuo. 59.8 g (87.7% of theory) of 5-acetamido-1-(2,3,5,6-tetrafluoro-4-trifluoromethyl-phenyl)-pyrazole of melting point 102° C. -104° C. are obtained.

후처리

  1. customrises from 20° C. to about 35° C
  2. customThe crystalline solid which has precipitated out
  3. filtrationis filtered off with suction
  4. washwashed freely with water and acetic acid
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-ab72b8dc8d414eb88c78b9936f291acc
출처 데이터셋
uspto-grants-1988_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04787930

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