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Water → HCID 9823111, 화합물

HRID 429326
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HRID 429326 반응식
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11](=O)[CH2:12][C:13](=O)[C:14]([F:17])([F:16])[F:15])=[CH:7][CH:6]=1)(=[O:4])=[O:3].Cl.[CH3:21][C:22]1[CH:23]=[C:24]([NH:29][NH2:30])[CH:25]=[CH:26][C:27]=1[Cl:28].O>C(O)(=O)C>[Cl:28][C:27]1[CH:26]=[CH:25][C:24]([N:29]2[C:11]([C:8]3[CH:9]=[CH:10][C:5]([S:2]([CH3:1])(=[O:4])=[O:3])=[CH:6][CH:7]=3)=[CH:12][C:13]([C:14]([F:17])([F:16])[F:15])=[N:30]2)=[CH:23][C:22]=1[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 15546184HCID 15546184, 화합물HCID 18355390(4-Chloro-3-methylphenyl)hydrazine--hydrogen chloride (1/1)

생성물 1

HCID 9823111HCID 9823111, 화합물수율 65.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 1-[4-(methylsulfonyl)phenyl]-4,4,4-trifluorobutane-1,3-dione (620 mg) and (3-methyl-4-chlorophenyl)hydrazine hydrochloride (425 mg) in acetic acid (2 ml) was refluxed for 1 hour. After cooling, the solvent was poured into water (50 ml) and stirred for 30 minutes. The resulting precipitates were collected by filtration and washed with water and dried in vacuo. The residue was recrystallized from ethanol to afford 1-(4-chloro-3-methylphenyl)-5-[4-(methylsulfonyl)phenyl]-3-(trifluoromethyl)pyrazole (569 mg).

후처리

  1. temperaturewas refluxed for 1 hour
  2. temperatureAfter cooling
  3. customThe resulting precipitates
  4. filtrationwere collected by filtration
  5. washwashed with water
  6. customdried in vacuo
  7. customThe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-15984ba194b54510ab8ea335f0a4c008
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06316485B1

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