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p-Toluenesulfonic acid → 3-Amino-1-(2-fluorobenzyl)-pyrazol-5-one

HRID 1605720
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인쇄 미리보기

반응식

HRID 1605720 반응식
C([O:3][C:4](=O)[CH:5]=[C:6]([NH2:10])OCC)C.C1(C)C=CC(S(O)(=O)=O)=CC=1.[F:23][C:24]1[CH:32]=[CH:31][CH:30]=[CH:29][C:25]=1[CH2:26][NH:27][NH2:28]>C(O)C>[NH2:10][C:6]1[NH:28][N:27]([CH2:26][C:25]2[CH:29]=[CH:30][CH:31]=[CH:32][C:24]=2[F:23])[C:4](=[O:3])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 278451beta-Aminobeta-ethoxyacrylic acid ethyl esterHCID 10374537(2-Fluorobenzyl)hydrazine

생성물 1

HCID 203673343-Amino-1-(2-fluorobenzyl)-pyrazol-5-one

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

30.2 g of β-amino-β-ethoxyacrylic acid ethyl ester together with 2 g of p-toluenesulphonic acid were dissolved in 300 ml of ethanol and 27.1 g of o-fluorobenzylhydrazine were added under nitrogen. After stirring for 2 hours, the mixture was left to stand overnight and the compound identified above, which had separated out as a precipitate, was filtered off and recrystallised from ethanol. Melting point: 146°, 11 g (27%).

후처리

  1. waitthe mixture was left
  2. waitto stand overnight
  3. customhad separated out as a precipitate
  4. filtrationwas filtered off
  5. customrecrystallised from ethanol

출처 및 근거

ORD 기록
ord-dc04bdb333de40a0b0bed98c1f8a5dd5
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03950528

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