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

HRID 621037
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HRID 621037 반응식
[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]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 178501737HCID 178501737, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-afc3671e31814279b264dca0a0fccbf0
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04822790

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