1-Bromo-2-butanone → 6-Bromo-2-ethylimidazo[1,2-a]pyridine

HRID 601666ノート

反応式

HRID 601666 の反応式
Br[CH2:2][C:3](=O)[CH2:4][CH3:5].[NH2:7][C:8]1[CH:13]=[CH:12][C:11]([Br:14])=[CH:10][N:9]=1>C(O)C>[Br:14][C:11]1[CH:12]=[CH:13][C:8]2[N:9]([CH:2]=[C:3]([CH2:4][CH3:5])[N:7]=2)[CH:10]=1

参加物

4

反応物 2

HCID 131561-Bromo-2-butanoneHCID 706222-Amino-5-bromopyridine

生成物 1

HCID 231582656-Bromo-2-ethylimidazo[1,2-a]pyridine収率 64.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5.0 g of 1-bromo-2-butanone was dissolved in 80 ml of ethanol, 5.71 g of 2-amino-5-bromopyridine was added, and the mixture was stirred all night by heating under reflux. After cooling down to room temperature, the solvents were distilled outunder reduced pressure, and ethyl acetated followed by saturated sodium bicarbonate aqueous solution were added. After drying organic layer with anhydrous sodium sulfate, the solvents were distilled outunder reduced pressure. The obtained residues were purified by preparative thin-layer silicagel chromatography (hexane:ethyl acetate=75:25), to obtain 4.82 g of the above compound as a white solid.

後処理

  1. temperatureby heating
  2. temperatureunder reflux
  3. distillationthe solvents were distilled outunder reduced pressure, and ethyl
  4. additionwere added
  5. dry with materialAfter drying organic layer with anhydrous sodium sulfate
  6. distillationthe solvents were distilled outunder reduced pressure
  7. customThe obtained residues were purified by preparative thin-layer silicagel chromatography (hexane:ethyl acetate=75:25)

出典と根拠

ORDレコード
ord-abd7cd04bb6643c68ca00741e741bc78
出典データセット
uspto-grants-2011_03
特許番号
US07902369B2

反応ノート

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