Potassium Carbonate → HCID 22727951, 화합물

HRID 2086070노트

반응식

HRID 2086070 반응식
[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5](Cl)=[N:6][CH:7]=1.[NH2:12][C:13]1[CH:14]=[C:15]([N:19]2[CH2:23][CH2:22][CH2:21][C:20]2=[O:24])[CH:16]=[CH:17][CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>ClCCCl.ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5]([NH:12][C:13]2[CH:14]=[C:15]([N:19]3[CH2:23][CH2:22][CH2:21][C:20]3=[O:24])[CH:16]=[CH:17][CH:18]=2)=[N:6][CH:7]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 6839561-(3-Aminophenyl)pyrrolidin-2-oneHCID 70194125-Bromo-2-chloro-3-nitropyridine

생성물 1

HCID 22727951HCID 22727951, 화합물수율 68%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 6344Dichloromethane용매

실험 절차

A suspension of 5-bromo-2-chloro-3-nitropyridine (3.79 g, 16 mmol), 1-(3-aminophenyl)pyrrolidin-2-one (2.56 g, 15 mmol) and potassium carbonate (2.0 g, 15 mmol) in 1,2-dichloroethane (25 ml) was heated at reflux for 60 hours. The reaction was cooled, diluted with dichloromethane (200 ml) and extracted with water. The organic phase was then dried over anhydrous sodium sulphate, filtered and pre-adsorbed on to silica (25 g). Purification by column chromatography eluting with isohexane on a gradient of ethyl acetate (10%-40%) gave 1-[3-(5-bromo-3-nitropyridin-2-ylamino)phenyl]pyrrolidin-2-one as a red solid (3.7 g, 68%).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 60 hours
  3. temperatureThe reaction was cooled
  4. extractionextracted with water
  5. dry with materialThe organic phase was then dried over anhydrous sodium sulphate
  6. filtrationfiltered and pre-adsorbed on to silica (25 g)
  7. customPurification by column chromatography
  8. washeluting with isohexane on a gradient of ethyl acetate (10%-40%)

출처 및 근거

ORD 기록
ord-802ee8b24a2c4f088055f85035af65ec
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06723735B1

반응 노트

불러오는 중…