Methyl acetoacetate → Methyl 1-acetylcyclopropane-1-carboxylate

HRID 83581노트

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HRID 83581 반응식
[C:1]([O:7][CH3:8])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].C(=O)([O-])[O-].[K+].[K+].Br[CH2:16][CH2:17]Br>CC(C)=O>[CH3:8][O:7][C:1]([C:2]1([C:3](=[O:4])[CH3:5])[CH2:17][CH2:16]1)=[O:6]

참가 물질

5

반응물 3

HCID 7757Methyl acetoacetateHCID 78391,2-DibromoethaneHCID 11430Potassium Carbonate

생성물 1

HCID 10214400Methyl 1-acetylcyclopropane-1-carboxylate

시약·촉매·용매 1

HCID 180Acetone용매

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온도
65 °C

실험 절차

To a solution of methyl acetoacetate (3 ml) in acetone (30 ml) were sequentially added potassium carbonate (11.54 g) and 1,2-dibromoethane (2.4 ml) at room temperature, and the mixture was stirred at 65° C. for 17 hours. This reaction mixture was filtered, the filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=10/1) to give the titled compound (2.17 g).

후처리

  1. customat room temperature
  2. filtrationThis reaction mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customthe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=10/1)

출처 및 근거

ORD 기록
ord-6de4f53d1c7c4a7686de67513f7896dc
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846746B2

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