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Vanillin → 2-hydroxy-N-[(E)-(4-hydroxy-3-methoxyphenyl)methylideneamino]-2-(4-methoxyphenyl)acetamide

HRID 458250
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HRID 458250 반응식
O=[CH:2][C:3]1[CH:11]=[CH:10][C:8]([OH:9])=[C:5]([O:6][CH3:7])[CH:4]=1.[OH:12][CH:13]([C:18]1[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=1)[C:14]([NH:16][NH2:17])=[O:15]>C(O)C>[OH:9][C:8]1[CH:10]=[CH:11][C:3](/[CH:2]=[N:17]/[NH:16][C:14](=[O:15])[CH:13]([OH:12])[C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)=[CH:4][C:5]=1[O:6][CH3:7]
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참가 물질

4

반응물 2

HCID 1183VanillinHCID 13479528Hydroxy-(4-methoxy-phenyl)-acetic acid hydrazide

생성물 1

HCID 1360285302-hydroxy-N-[(E)-(4-hydroxy-3-methoxyphenyl)methylideneamino]-2-(4-methoxyphenyl)acetamide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Vanillin (23 g, 0.15 mol) is added to a solution of hydroxy-(4-methoxy-phenyl)-acetic acid hydrazide (30 g, 0.15 mol) in 300 ml of ethanol at room temperature. After heating this mixture to reflux for 4 hours, the reaction is poured on water and extracted with ethyl acetate. The combined organic layer is washed with brine, dried over magnesium sulfate and evaporated. The residue, which is hydroxy-(4-methoxy-phenyl)-acetic acid [1-(4-hydroxy-3-methoxy-phenyl)-meth-(E)-ylidene]-hydrazide, is sufficiently pure to be directly used in the next step.

후처리

  1. temperatureAfter heating this mixture
  2. temperatureto reflux for 4 hours
  3. additionthe reaction is poured on water
  4. extractionextracted with ethyl acetate
  5. washThe combined organic layer is washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated

출처 및 근거

ORD 기록
ord-7c7168e3a55c4c46aa54477a64b1fe86
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07189873B2

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