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Hydrochloric Acid → 5-(3,4-Dimethoxyphenyl)-5-oxovaleric acid

HRID 1757642
ノート
印刷プレビュー

反応式

HRID 1757642 の反応式
[C:1]1([O:9][CH3:10])[C:2](=[CH:5][CH:6]=[CH:7][CH:8]=1)[O:3][CH3:4].[C:11]1(=[O:18])[O:17][C:15](=[O:16])[CH2:14][CH2:13][CH2:12]1.[Cl-].[Al+3].[Cl-].[Cl-].Cl>[N+](C1C=CC=CC=1)([O-])=O>[CH3:4][O:3][C:2]1[CH:5]=[C:6]([C:11](=[O:18])[CH2:12][CH2:13][CH2:14][C:15]([OH:17])=[O:16])[CH:7]=[CH:8][C:1]=1[O:9][CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7043VeratroleHCID 7940Glutaric anhydrideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 27584705-(3,4-Dimethoxyphenyl)-5-oxovaleric acid

試薬・触媒・溶媒 1

HCID 7416Nitrobenzene溶媒2 回

実験手順

A solution containing 36 g of veratrole and 30 g glutaric anhydride in 120 ml of nitrobenzene was gradually added while stirring and cooling at 0° C. to a mixture of 72 g of anhydrous aluminium chloride and 240 ml of nitrobenzene. The mixture was stirred for 1 h at 0° C. and then for 18 h at 20° C. Ice and hydrochloric acid were added to thereaction mixture. Nitrobenzene layer was separated and to this ethyl acetate was added whereupon the product crystallized. After filtering the crystals were washed with ethyl acetate. Yield 42.3 g (64%).

後処理

  1. additionwas gradually added
  2. stirringThe mixture was stirred for 1 h at 0° C.
  3. customNitrobenzene layer was separated and to this ethyl acetate
  4. additionwas added whereupon the product
  5. customcrystallized
  6. filtrationAfter filtering the crystals
  7. washwere washed with ethyl acetate

出典と根拠

ORDレコード
ord-34465f480b5543bdb181c03238c8cf40
出典データセット
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05446194

反応ノート

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