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Acetic Acid → Diethyl 2-(3,4-dimethoxybenzylidene)malonate

HRID 424605
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인쇄 미리보기

반응식

HRID 424605 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=O.[CH2:13]([O:15][C:16](=[O:23])[CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH3:14].C(O)(=O)C.N1CCCCC1>C1C=CC=CC=1.O>[CH2:13]([O:15][C:16](=[O:23])[C:17](=[CH:6][C:5]1[CH:8]=[CH:9][C:10]([O:11][CH3:12])=[C:3]([O:2][CH3:1])[CH:4]=1)[C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 7761Diethyl MalonateHCID 8082PiperidineHCID 8419Veratraldehyde

생성물 1

HCID 335552Diethyl 2-(3,4-dimethoxybenzylidene)malonate

시약·촉매·용매 2

HCID 241Benzene용매HCID 962
Water
용매
2회

실험 절차

3,4-dimethoxybenzaldehyde (Veratraldehyde) (9.13 g, 55 mM) was heated with malonic acid diethyl ester (8.00 g, 50 mM), acetic acid (0.29 ml) and piperidine (0.74 ml) in benzene (100 ml) in an apparatus equipped with a water separator (Dean-Stark tube) until 50 mM water was separated. After washing the benzene solution with water, it was dried over anhydrous magnesium sulfate. After drying, benzene was evaporated under reduced pressure to obtain a crude product (15.40 g). The crude product thus obtained is pure enough, and can be used in the subsequent reaction without further purification.

후처리

  1. customwas separated
  2. washAfter washing the benzene solution with water, it
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. customAfter drying
  5. custombenzene was evaporated under reduced pressure
  6. customto obtain a crude product (15.40 g)

출처 및 근거

ORD 기록
ord-47ee0ab220f04305ba10fa44f3dc9857
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08106053B2

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