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

HRID 856791
ノート
印刷プレビュー

反応式

HRID 856791 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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)

出典と根拠

ORDレコード
ord-68b93a7fe6e043de8a1542c6384c7cbb
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262185B2

反応ノート

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