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(4-Methylphenyl)hydrazine → 5-Pentafluoroethyl-2-p-tolyl-2H-pyrazol-3-ylamine

HRID 729596
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인쇄 미리보기

반응식

HRID 729596 반응식
[F:1][C:2]([F:12])([C:8]([F:11])([F:10])[F:9])[C:3](=O)[CH2:4][C:5]#[N:6].[C:13]1([CH3:21])[CH:18]=[CH:17][C:16]([NH:19][NH2:20])=[CH:15][CH:14]=1>C(O)C>[F:1][C:2]([F:12])([C:3]1[CH:4]=[C:5]([NH2:6])[N:19]([C:16]2[CH:17]=[CH:18][C:13]([CH3:21])=[CH:14][CH:15]=2)[N:20]=1)[C:8]([F:9])([F:11])[F:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10875(4-Methylphenyl)hydrazineHCID 156138214,4,5,5,5-Pentafluoro-3-oxopentanenitrile

생성물 1

HCID 578328135-Pentafluoroethyl-2-p-tolyl-2H-pyrazol-3-ylamine수율 52%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Heat a mixture of 4,4,5,5,5-pentafluoro-3-oxo-pentanenitrile (4 g, 21.4 mmol) and p-tolyl-hydrazine (10 g, 64.1 mmol) in ethanol (20 mL) to 95° C. in a sealed tube apparatus for 15 hours. After cooling to room temperature, remove the solvent under reduced pressure to give a brown residue. Subject residue to silica gel chromatography eluting with ethyl acetate and hexanes to give the title compound (3.24 g, 52% yield, ES+(m/z) 292.1 [M+H]).

후처리

  1. temperatureHeat
  2. customremove the solvent under reduced pressure
  3. customto give a brown residue
  4. washSubject residue to silica gel chromatography eluting with ethyl acetate and hexanes

출처 및 근거

ORD 기록
ord-68bcfd48251b4a368446c3d13389209c
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582638B2

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