2-Butanone, 3-bromo- → Ethyl 8-amino-2,3-dimethylimidazo[1,2-a]pyridine-6-carboxylate

HRID 427502노트

반응식

HRID 427502 반응식
[NH2:1][C:2]1[C:3]([NH2:13])=[N:4][CH:5]=[C:6]([CH:12]=1)[C:7]([O:9][CH2:10][CH3:11])=[O:8].Br[CH:15]([CH3:19])[C:16](=O)[CH3:17]>COCCOC>[NH2:1][C:2]1[C:3]2[N:4]([C:15]([CH3:19])=[C:16]([CH3:17])[N:13]=2)[CH:5]=[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH:12]=1

참가 물질

4

반응물 2

HCID 131422-Butanone, 3-bromo-HCID 9877541Ethyl 5,6-diaminonicotinate

생성물 1

HCID 9942738Ethyl 8-amino-2,3-dimethylimidazo[1,2-a]pyridine-6-carboxylate수율 17.9%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

Ethyl 5,6-diaminonicotinate (1.4 g, 7.7 mmol) and 3-bromo-2-butanon (1.16 g, 7.2 mmol) were added to 1,2-dimethoxyethan (50 ml) and refluxed for 20 h. The solvent was evaporated under reduced pressure and the residue was dissolved in methylene chloride. The methylene chloride solution was washed with saturated sodium bicarbonate and dried (Na2SO4). The solvent was evaporated under reduced pressure and the residue was purified by column chromatography on silica gel using methylene chloride:methanol (10:1) as eluent to give 0.3 g (17%) of the title compound.

후처리

  1. temperaturerefluxed for 20 h
  2. customThe solvent was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in methylene chloride
  4. washThe methylene chloride solution was washed with saturated sodium bicarbonate
  5. dry with materialdried (Na2SO4)
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-b89a31684d71434fa2939fd30ddbf065
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313137B1

반응 노트

불러오는 중…