Water → HCID 23143553、化合物

HRID 1437269

反応式

HRID 1437269 の反応式
[C:1]([O:7][CH3:8])(=[O:6])[C:2]([O:4]C)=O.[CH3:9][O-].[Na+].[Cl:12][C:13]1[CH:14]=[CH:15][C:16]([C:19](=[O:21])[CH3:20])=[N:17][CH:18]=1.O>C(O)C>[CH2:8]([O:7][C:1](=[O:6])[C:2](=[O:4])[CH2:20][C:19]([C:16]1[CH:15]=[CH:14][C:13]([Cl:12])=[CH:18][N:17]=1)=[O:21])[CH3:9]

参加物

6

反応物 4

HCID 962WaterHCID 11120Dimethyl oxalateHCID 101541661-(5-Chloropyridin-2-yl)ethan-1-oneHCID 10942334Sodium Methoxide

生成物 1

HCID 23143553HCID 23143553、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dimethyl oxalate (5 g) was added to sodium methoxide (2.26 g) in ethanol (100 mL), and the mixture was stirred for 5 minutes. 1-(5-Chloro-2-pyridyl)ethanone (3.26 g) was added to the mixture, followed by stirring at room temperature for 45 minutes. Water was added to the reaction mixture, and the resultant mixture was washed with diethyl ether. The aqueous layer was acidified with aqueous 1N hydrochloric acid, and chloroform was added thereto to partition the mixture. The organic layer was dried over sodium sulfate anhydrate, followed by filtration. The solvent was removed under reduced pressure, to thereby give 4-(5-chloro-2-pyridyl)-2,4-dioxobutanoic acid ethyl ester as a solid (4.12 g, 77%).

後処理

  1. stirringby stirring at room temperature for 45 minutes
  2. washthe resultant mixture was washed with diethyl ether
  3. additionwas added
  4. customto partition the mixture
  5. dry with materialThe organic layer was dried over sodium sulfate anhydrate
  6. filtrationfollowed by filtration
  7. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-48ec55115d154f598dc0667b85098c9d
出典データセット
uspto-grants-2009_11
特許番号
US07622471B2

関連ノート

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