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Potassium Carbonate → ethyl (2-formyl-1H-imidazol-1-yl)acetate

HRID 856791
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HRID 856791 반응식
[CH:1]([C:3]1[NH:4][CH:5]=[CH:6][N:7]=1)=[O:2].[C:8]([O:11][CH2:12][CH2:13]Br)(=[O:10])[CH3:9].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH:1]([C:3]1[N:4]([CH2:9][C:8]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][N:7]=1)=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 249551H-imidazole-2-carbaldehyde

생성물 1

HCID 62222097ethyl (2-formyl-1H-imidazol-1-yl)acetate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2-formylimidazole (5.16 g), bromoethyl acetate (7.1 ml) and potassium carbonate (11.1 g) in. DMF (50 ml) was stirred for 20 hours at 60° C. The insolubles were removed by filtration, water was added to the mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The obtained residue was separated and purified by column chromatography (ethyl acetate:hexane 1:1), to give ethyl (2-formyl-1H-imidazol-1-yl)acetate (1.10 g) as pale yellow oil.

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후처리

  1. customThe insolubles were removed by filtration, water
  2. additionwas added to the mixture
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained residue was separated
  8. custompurified by column chromatography (ethyl acetate:hexane 1:1)

출처 및 근거

ORD 기록
ord-68b93a7fe6e043de8a1542c6384c7cbb
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07262185B2

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