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

HRID 424605
ノート
印刷プレビュー

反応式

HRID 424605 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 7761Diethyl MalonateHCID 8082PiperidineHCID 8419Veratraldehyde

生成物 1

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

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 962
Water
溶媒
2 回

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-47ee0ab220f04305ba10fa44f3dc9857
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08106053B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート