Hydrochloric Acid → HCID 68677988, 화합물

HRID 1993924노트

반응식

HRID 1993924 반응식
CO[C:3](=[O:16])[CH2:4][C:5](=O)[CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=1.[F:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][NH2:25])=[CH:20][CH:19]=1.Cl.CCOC(C)=O>C(O)(=O)C.O>[F:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]2[C:3](=[O:16])[CH2:4][C:5]([CH2:6][CH2:7][C:8]3[CH:9]=[CH:10][C:11]([F:14])=[CH:12][CH:13]=3)=[N:25]2)=[CH:20][CH:19]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 69982(4-Fluorophenyl)hydrazineHCID 66789979500367-64-6

생성물 1

HCID 68677988HCID 68677988, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

To a solution of 5-(4-fluoro-phenyl)-3-oxo-pentanoic acid methyl ester (0.43 g) in acetic acid (5 mL) in a sealable tube was added 4-fluorophenylhydrazine.HCl (0.31 g). The reaction vessel was sealed and immersed into an oil bath at 100° C. for 18 hours. The reaction vessel was cooled to ambient temperature, opened and the contents were poured onto a mixture of EtOAc and water. The aqueous phase was extracted with EtOAc and the combined organic phases were washed with water and dried over sodium sulfate. Filtration and evaporation of the volatiles in vacuo afforded a crude crystalline material. The crude product was washed with ether to afford the desired 2-(4-fluoro-phenyl)-5-[2-(4-fluoro-phenyl)-ethyl]-2,4-dihydro-pyrazol-3-one (0.37 g) as a beige crystalline solid. MS (ESI+): 301.1 [M+H]+).

후처리

  1. customThe reaction vessel was sealed
  2. extractionThe aqueous phase was extracted with EtOAc
  3. washthe combined organic phases were washed with water
  4. dry with materialdried over sodium sulfate
  5. filtrationFiltration and evaporation of the volatiles in vacuo
  6. customafforded a crude crystalline material
  7. washThe crude product was washed with ether

출처 및 근거

ORD 기록
ord-00157bec1a6a4e4b8037323192c2c75b
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07652057B2

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