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

HRID 601645노트

반응식

HRID 601645 반응식
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

참가 물질

4

반응물 2

HCID 21642BromopinacoloneHCID 706222-Amino-5-bromopyridine

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-7fc6e1ddfaa341028f309c772b7d2bde
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902369B2

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