Bromopinacolone → 6-Bromo-2-tert-butylimidazo[1,2-a]pyridine

HRID 601645ノート

反応式

HRID 601645 の反応式
Br[CH2:2][C:3](=O)[C:4]([CH3:7])([CH3:6])[CH3:5].[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([Br:16])=[CH:12][N:11]=1>C(O)C>[Br:16][C:13]1[CH:14]=[CH:15][C:10]2[N:11]([CH:2]=[C:3]([C:4]([CH3:7])([CH3:6])[CH3:5])[N:9]=2)[CH:12]=1

参加物

4

反応物 2

HCID 21642BromopinacoloneHCID 706222-Amino-5-bromopyridine

生成物 1

HCID 231582386-Bromo-2-tert-butylimidazo[1,2-a]pyridine収率 81.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-bromopinacolone (178 mg) was dissolved in 2.0 ml of ethanol, 156 mg of 2-amino-5-bromopyridine was added, and the mixture was stirred all night by heating under reflux. After cooled down to room temperature, the solvents were distilled outunder reduced pressure, ethyl acetate followed by saturated sodium hydrogen carbonate aqueous solution were added. Organic layer was dried with anhydrous sodium sulfate, and 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 186 mg 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, ethyl acetate
  4. additionwere added
  5. dry with materialOrganic layer was dried 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-7fc6e1ddfaa341028f309c772b7d2bde
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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