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

HRID 1977693
ノート
印刷プレビュー

反応式

HRID 1977693 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.[C:13]([O:21][CH2:22][CH3:23])(=[O:20])[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16].C(O)(=O)C.N1CCCCC1>C1C=CC=CC=1.O>[CH2:18]([O:17][C:15](=[O:16])[C:14](=[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:13]([O:21][CH2:22][CH3:23])=[O:20])[CH3:19]
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

9.13 g (55 mM) of 3,4-Dimethoxybenzaldehyde (veratraldehyde) was heated in 100 ml of benzene together with 8.00 mg (50 mM) of diethyl malonate, 0.29 ml of acetic acid, and 0.74 ml of piperidine in an apparatus equipped with a water separation tube (i.e., Dean Stark tube) until 50 mM water was separated. The benzene solution was washed with water and was dried over anhydrous magnesium sulfate. After being dried, the benzene was evaporated in vacuo to obtain 15.40 g crude product. The crude product obtained here had a sufficient purity even without purification, thus could be used as it was in the following step.

後処理

  1. customwas separated
  2. washThe benzene solution was washed with water
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. customAfter being dried
  5. customthe benzene was evaporated in vacuo
  6. customto obtain 15.40 g crude product

出典と根拠

ORDレコード
ord-c333055e3d12404db6b0ff9f4ee6f81a
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06235739B1

反応ノート

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