Methyl acetoacetate → Methyl 1-acetylcyclopropane-1-carboxylate

HRID 1790876노트

반응식

HRID 1790876 반응식
[CH3:1][O:2][C:3](=[O:8])[CH2:4][C:5]([CH3:7])=[O:6].C(=O)([O-])[O-].[K+].[K+].Br[CH:16](Br)[CH3:17]>CC(C)=O.C(OCC)(=O)C>[CH3:1][O:2][C:3]([C:4]1([C:5](=[O:6])[CH3:7])[CH2:17][CH2:16]1)=[O:8]

참가 물질

6

반응물 3

HCID 7757Methyl acetoacetateHCID 112011,1-DibromoethaneHCID 11430Potassium Carbonate

생성물 1

HCID 10214400Methyl 1-acetylcyclopropane-1-carboxylate

시약·촉매·용매 2

HCID 180Acetone용매HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

56 g of acetoacetic acid methyl ester 3 is dissolved in 500 ml of acetone, and 276.2 g of potassium carbonate as well as 86 ml of dibromoethane are added while being cooled with ice. It is heated under nitrogen to 50° C. and stirred for 72 hours at this temperature. After cooling, the mixture is diluted with ethyl acetate, washed with water and saturated sodium chloride solution, dried on sodium sulfate and concentrated by evaporation. The residue is distilled in a vacuum, whereby 66 g of the title compound is obtained as a colorless oil.

후처리

  1. temperaturewhile being cooled with ice
  2. temperatureAfter cooling
  3. washwashed with water and saturated sodium chloride solution
  4. customdried on sodium sulfate
  5. concentrationconcentrated by evaporation
  6. distillationThe residue is distilled in a vacuum

출처 및 근거

ORD 기록
ord-288b99af453e4009bbf2075cf217e681
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07071344B1

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