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Hydrazine hydrate (1:1) → 2,3-Dichloro-4-trifluoromethyl-phenylhydrazine

HRID 2107883
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HRID 2107883 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6](Cl)[CH:5]=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11].O.[NH2:15][NH2:16]>N1C=CC=CC=1>[Cl:8][C:7]1[C:2]([Cl:1])=[C:3]([C:10]([F:13])([F:12])[F:11])[CH:4]=[CH:5][C:6]=1[NH:15][NH2:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 133082441,2,3-Trichloro-4-(trifluoromethyl)benzene

생성물 1

HCID 139134182,3-Dichloro-4-trifluoromethyl-phenylhydrazine수율 80%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

100 g (0.4 mol) of 2,3,4-trichlorobenzotrifluoride are initially introduced, 200 ml of pyridine and subsequently 100 g (2.0 mol) of hydrazine hydrate are added, and the mixture is then heated to the reflux temperature for 12 hours. 90% of the pyridine is then removed by distillation, and the residue remaining is stirred into 250 ml of water. The crystalline product is filtered off with suction, washed with some water and dried. 78 g (80% of theory) of 2,3-dichloro-4-trifluoromethyl-phenylhydrazine of melting point 79° to 80° C. are obtained.

후처리

  1. temperaturethe mixture is then heated to the reflux temperature for 12 hours
  2. custom90% of the pyridine is then removed by distillation
  3. filtrationThe crystalline product is filtered off with suction
  4. washwashed with some water
  5. customdried

출처 및 근거

ORD 기록
ord-9c5f362dd5d644d8b11057adfd09559e
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04936892

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