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Hydrochloric Acid → 4,4'-dimethoxybenzophenone O-(3-ethoxycarbonyl-2-oxopropyl)oxime

HRID 1029787
ノート
印刷プレビュー

反応式

HRID 1029787 の反応式
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([C:7](=[N:16][OH:17])[C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.CC(C)([O-])C.[K+].Cl[CH2:27][C:28](=[O:35])[CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31].Cl>CN(C)C=O>[CH2:33]([O:32][C:30]([CH2:29][C:28](=[O:35])[CH2:27][O:17][N:16]=[C:7]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=1)[C:6]1[CH:18]=[CH:19][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)=[O:31])[CH3:34]
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 69484Ethyl 4-chloroacetoacetateHCID 289718n-Hydroxy-1,1-bis(4-methoxyphenyl)methanimine2 回HCID 23665647Potassium tert-butoxide

生成物 1

HCID 140527694,4'-dimethoxybenzophenone O-(3-ethoxycarbonyl-2-oxopropyl)oxime収率 80.4%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

2.57 g (0.01 mol) of the 4,4'-dimethoxybenzophenone oxime as obtained in (1) was dissolved in 5 ml of dimethylformamide and 1.2 g of potassium tert-butoxide was added thereto under ice cooling. The resulting mixture was stirred for ten minutes. Then 1.8 g of ethyl 4-chloroacetoacetate was added thereto and the obtained mixture was stirred at room temperature. After two hours, the reaction mixture was poured into diluted hydrochloric acid and extracted with ethanol. The crude product thus obtained was purified by silica gel chromatography to give 3.1 g of the title compound.

後処理

  1. stirringthe obtained mixture was stirred at room temperature
  2. extractionextracted with ethanol
  3. customThe crude product thus obtained
  4. customwas purified by silica gel chromatography

出典と根拠

ORDレコード
ord-15df401373dc48789f51b3c58cf341e0
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05103010

反応ノート

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