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Vanillin → 3-(4-Hydroxy-3-methoxyphenyl)-1-(4-hydroxyphenyl)prop-2-en-1-one

HRID 883439
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HRID 883439 반응식
[OH-].[K+].[OH:3][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:12])[CH3:11])=[CH:6][CH:5]=1.O=[CH:14][C:15]1[CH:23]=[CH:22][C:20]([OH:21])=[C:17]([O:18][CH3:19])[CH:16]=1>C(OCCOCCOCC)C>[OH:21][C:20]1[CH:22]=[CH:23][C:15]([CH:14]=[CH:11][C:10]([C:7]2[CH:8]=[CH:9][C:4]([OH:3])=[CH:5][CH:6]=2)=[O:12])=[CH:16][C:17]=1[O:18][CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1183VanillinHCID 74694'-HydroxyacetophenoneHCID 14797Potassium Hydroxide

생성물 1

HCID 667388783-(4-Hydroxy-3-methoxyphenyl)-1-(4-hydroxyphenyl)prop-2-en-1-one수율 93.8%

시약·촉매·용매 1

HCID 8179Diethylene glycol diethyl ether용매

실험 절차

Potassium hydroxide (20 g) in 100 g of diethylene glycol diethyl ether is heated to 120° C. while being stirred, and added to a mixture of 14 g of p-hydroxyacetophenone and 15 g of vanillin within 1 h. Upon completion of the addition stirring is continued for another 20 min., a hydrolysis is carried out and the pH is adjusted to 6-7. After phase separation, the solvent is removed and 25 g of 3-(4-hydroxy-3-methoxyphenyl)-1-(4-hydroxyphenyl)-2-propene-1-one is obtained. Yield: 93% of the theory.

후처리

  1. additionUpon completion of the addition
  2. stirringstirring
  3. customAfter phase separation
  4. customthe solvent is removed

출처 및 근거

ORD 기록
ord-4a69c4a32cfa4679b441d30a28ee7b17
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08236859B2

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