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Water → Methyl 4-cyano-3-oxobutanoate

HRID 1837321
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HRID 1837321 반응식
[C-:1]#[N:2].[K+].Cl[CH2:5][C:6](=[O:12])[CH2:7][C:8]([O:10][CH3:11])=[O:9].O>CO.S(=O)(=O)(O)O>[C:1]([CH2:5][C:6](=[O:12])[CH2:7][C:8]([O:10][CH3:11])=[O:9])#[N:2]
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참가 물질

6

반응물 3

HCID 962WaterHCID 9032Potassium CyanideHCID 36240Methyl 4-chloroacetoacetate

생성물 1

HCID 9964118Methyl 4-cyano-3-oxobutanoate수율 69.2%

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 887Methanol용매

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온도
40 °C

실험 절차

After 0.4 g of potassium cyanide was added at room temperature to a solution of 1 g of Methyl 4-chloro-3-oxobutanoate in 20 ml of methanol, the resulting mixture was warmed to 40° C. and maintained for further 8 hours. Thereafter, reaction solution was cooled and pH of the solution was adjusted to 3 by adding 10 ml of water and a few drops of concentrated sulfuric acid. After the mixture was extracted thrice with diethyl ether, total amount of which was 100 ml, the separated organic layers were combined and concentrated under reduced pressure to give 0.6 g of methyl 4-cyano-3-oxobutanoate (Purity: 71%).

후처리

  1. temperaturemaintained for further 8 hours
  2. customThereafter, reaction solution
  3. temperaturewas cooled
  4. extractionAfter the mixture was extracted thrice with diethyl ether, total amount of which
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0bbd713c8be34d339bac4ee9bd7ed0f1
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06781009B2

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