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Potassium Carbonate → 2-(n-Propoxyimino)acetoacetic acid methyl ester

HRID 465238
ノート
印刷プレビュー

反応式

HRID 465238 の反応式
[CH3:1][O:2][C:3](=[O:10])[C:4](=[N:8][OH:9])[C:5]([CH3:7])=[O:6].C(=O)([O-])[O-].[K+].[K+].[CH2:17](I)[CH2:18][CH3:19]>CC(C)=O>[CH3:1][O:2][C:3](=[O:10])[C:4](=[N:8][O:9][CH2:17][CH2:18][CH3:19])[C:5]([CH3:7])=[O:6]
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 11430Potassium CarbonateHCID 336431-IodopropaneHCID 178501737HCID 178501737、化合物

生成物 1

HCID 542075682-(n-Propoxyimino)acetoacetic acid methyl ester収率 80%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 13.6 g of 2-hydroxyiminoacetoacetic acid methyl ester in 70 ml of acetone is added under ice cooling 20.8 g of potassium carbonate. To the mixture is added dropwise 17.0 g of n-propyl iodide in the course of 30 minutes. At the end of the dropwise addition, the mixture is stirred at room temperature for 2 hours. Acetone is evaporated under reduced pressure. To the residue is added 250 ml of water, and the mixture is subjected to extraction with methylene chloride. The extract is washed with water twice, dried over anhydrous sodium sulfate, followed by evaporation of the solvent under reduced pressure to yield 2-(n-propoxyimino)acetoacetic acid methyl ester as a pale yellow oily product.

後処理

  1. additionAt the end of the dropwise addition
  2. customAcetone is evaporated under reduced pressure
  3. additionTo the residue is added 250 ml of water
  4. extractionthe mixture is subjected to extraction with methylene chloride
  5. washThe extract is washed with water twice
  6. dry with materialdried over anhydrous sodium sulfate
  7. customfollowed by evaporation of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-c0a29b2fab8d4e67bae31d614f3a9483
出典データセット
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04550105

反応ノート

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