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3,4,5-Trimethoxybenzaldehyde → Trimethoxybenzylidene pentanedione

HRID 1915991
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반응식

HRID 1915991 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:13][CH3:14])[C:10]=1[O:11][CH3:12])[CH:6]=O.[C:15]([CH2:18][C:19](=[O:21])[CH3:20])(=[O:17])[CH3:16].N1CCCCC1>C1CCCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:13][CH3:14])[C:10]=1[O:11][CH3:12])[CH:6]=[C:18]([C:19](=[O:21])[CH3:20])[C:15](=[O:17])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 68583,4,5-TrimethoxybenzaldehydeHCID 8082PiperidineHCID 31261Acetylacetone

생성물 1

HCID 67772502Trimethoxybenzylidene pentanedione

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

3-(3,4,5-trimethoxybenzylidene)-2,4-pentanedione (hereinafter “HSS”) was prepared by the condensation of 3,4,5-trimethoxy 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. The typical yield of HSS is about 68% with a purity, as determined by GC, of 99.1%. HSS is an off-white free-flowing powder with a melting point of 83-86° 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-72946f87abbe4ad595c6c987876149ea
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08617528B2

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