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Acetic Acid → 4-(3,4-Dimethoxyphenyl)but-3-en-2-one

HRID 1108752
ノート
印刷プレビュー

反応式

HRID 1108752 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.N1CC[CH2:16][CH2:15][CH2:14]1.C(O)(=[O:21])C>CC(C)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]=[CH:14][C:15](=[O:21])[CH3:16])[CH:8]=[CH:9][C:10]=1[O:11][CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 176Acetic AcidHCID 8082PiperidineHCID 8419Veratraldehyde

生成物 1

HCID 847484-(3,4-Dimethoxyphenyl)but-3-en-2-one収率 56.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

3,4-Dimethoxybenzaldehyde (30.1 g) was dissolved in acetone (900 ml), and then piperidine (23.2 ml) and acetic acid (13.4 ml) were added prior to reflux for 4 hours. After distilling off the reaction solvent under reduced pressure, it was dissolved in 600 ml of ethyl acetate and washed with saturated sodium bicarbonate water and saturated saline. After drying with anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure producing yellow crystals which were then washed in isopropyl ether to give 21.0 g of 4-(3,4-dimethoxyphenyl)-3-buten-2-one (56.4%).

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

後処理

  1. temperatureto reflux for 4 hours
  2. distillationAfter distilling off the reaction solvent under reduced pressure, it
  3. dissolutionwas dissolved in 600 ml of ethyl acetate
  4. washwashed with saturated sodium bicarbonate water and saturated saline
  5. dry with materialAfter drying with anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customproducing yellow crystals which
  8. washwere then washed in isopropyl ether

出典と根拠

ORDレコード
ord-642f1bf43dfa4cbc9dbefaaeb23d6818
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06069176

反応ノート

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