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Water → Ethyl 4-(4-methyl-2-pyridyl)-2,4-dioxobutanoate

HRID 1437274
ノート
印刷プレビュー

反応式

HRID 1437274 の反応式
[C:1]([O:8][CH2:9][CH3:10])(=[O:7])[C:2]([O:4]CC)=O.[O-]CC.[Na+].[CH3:15][C:16]1[CH:21]=[CH:20][N:19]=[C:18]([C:22](=[O:24])[CH3:23])[CH:17]=1.O>C(O)C>[CH2:9]([O:8][C:1](=[O:7])[C:2](=[O:4])[CH2:23][C:22]([C:18]1[CH:17]=[C:16]([CH3:15])[CH:21]=[CH:20][N:19]=1)=[O:24])[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 962WaterHCID 7268Diethyl OxalateHCID 5647602-Acetyl-4-methylpyridineHCID 2723922Sodium ethoxide

生成物 1

HCID 23143392Ethyl 4-(4-methyl-2-pyridyl)-2,4-dioxobutanoate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Diethyl oxalate (4.42 mL) was added to sodium ethoxide (2.22 g) in ethanol (22 mL), and the mixture was stirred for 10 minutes. The above-obtained 1-(4-methyl-2-pyridyl)ethanone (2.20 g) in ethanol (22 mL) was added to the mixture, followed by stirring at room temperature for 20 minutes. Water was added to the reaction mixture, and the resultant mixture was washed with diethyl ether, and then the aqueous layer was partitioned by use of saturated aqueous ammonium chloride and chloroform. The organic layer was dried over sodium sulfate anhydrate, followed by filtration. The solvent was removed under reduced pressure, to thereby give 4-(4-methyl-2-pyridyl)-2,4-dioxobutanoic acid ethyl ester as an oily product (2.84 g, 74%).

後処理

  1. stirringby stirring at room temperature for 20 minutes
  2. washthe resultant mixture was washed with diethyl ether
  3. customthe aqueous layer was partitioned by use of saturated aqueous ammonium chloride and chloroform
  4. dry with materialThe organic layer was dried over sodium sulfate anhydrate
  5. filtrationfollowed by filtration
  6. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-dd086131303447cfb627f7c756da0cb3
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07622471B2

反応ノート

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