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Piperidine → 3-(4-Methoxybenzylidene)pentane-2,4-dione

HRID 1915993
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HRID 1915993 반응식
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=O)=[CH:5][CH:4]=1.[C:11]([CH2:14][C:15](=[O:17])[CH3:16])(=[O:13])[CH3:12].N1CCCCC1>C1CCCCC1>[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[C:14]([C:15](=[O:17])[CH3:16])[C:11](=[O:13])[CH3:12])=[CH:5][CH:4]=1
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참가 물질

5

반응물 3

HCID 8082PiperidineHCID 312444-MethoxybenzaldehydeHCID 31261Acetylacetone

생성물 1

HCID 2404143-(4-Methoxybenzylidene)pentane-2,4-dione수율 70%

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

3-(4-methoxybenzylidene)-2,4-pentanedione was prepared by the condensation of 4-methoxy benzaldehyde with acetyl acetone in the presence of piperidine and cyclohexane as the reaction medium at reflux temperature under continuous azeotropic water removal. The reaction takes about eight hours to complete. The reaction product was purified by crystallization with methanol and yields about 70% 3-(4-methoxybenzylidene)-2,4-pentanedione (hereinafter “Compound 3”) with a purity, as determined by GC, of about 99.6%. Compound 3 is an off-white free-flowing powder having a melting point of 82-84° C. with a λmax at 319 nm.

후처리

  1. temperatureat reflux temperature under continuous azeotropic water
  2. customremoval
  3. customThe reaction product was purified by crystallization with methanol

출처 및 근거

ORD 기록
ord-47be98813c9942f79417580fca1170b1
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08617528B2

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