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Dimethylformamide → 1-Phenyl-4-pyridin-4-yl-1,2-dihydro-3H-pyrazol-3-one

HRID 1867613
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인쇄 미리보기

반응식

HRID 1867613 반응식
[C:1]1([NH:7][NH:8][C:9](=[O:17])[CH2:10][C:11]2[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Ca+2].[H-].[CH3:21]N(C)C=O>>[C:1]1([N:7]2[CH:21]=[C:10]([C:11]3[CH:12]=[CH:13][N:14]=[CH:15][CH:16]=3)[C:9](=[O:17])[NH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 3033859Calcium hydrideHCID 68566518N'-phenyl-2-pyridin-4-ylacetohydrazide

생성물 1

HCID 685657321-Phenyl-4-pyridin-4-yl-1,2-dihydro-3H-pyrazol-3-one

반응 조건

온도
170 °C

실험 절차

N′-Phenyl-2-pyridin-4-ylacetohydrazide (460 mg, 2.02 mmol) and calcium hydride (141 mg, 3.34 mmol) were dissolved in dimethylformamide (8 mL) and heated at 170° C. After 8 h, the reaction cooled to ambient temperature and was filtered. The mixture was concentrated and redissolved in dichloromethane (50 mL). The precipitate was filtered and dried under high vacuum overnight to give the desired product. MS 238.04 (M+1)

후처리

  1. temperaturethe reaction cooled to ambient temperature
  2. filtrationwas filtered
  3. concentrationThe mixture was concentrated
  4. dissolutionredissolved in dichloromethane (50 mL)
  5. filtrationThe precipitate was filtered
  6. customdried under high vacuum overnight

출처 및 근거

ORD 기록
ord-a85efc9bfcc4478b836216ff1275ae5d
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07632832B2

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