Pyridine → Ethyl N-(6,7-difluoro-2-methoxyquinoxalin-3-yl)carbamate

HRID 1878275

반응식

HRID 1878275 반응식
[NH2:1][C:2]1[C:11]([O:12][CH3:13])=[N:10][C:9]2[C:4](=[CH:5][C:6]([F:15])=[C:7]([F:14])[CH:8]=2)[N:3]=1.Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18].N1C=CC=CC=1>ClCCl>[F:15][C:6]1[CH:5]=[C:4]2[C:9](=[CH:8][C:7]=1[F:14])[N:10]=[C:11]([O:12][CH3:13])[C:2]([NH:1][C:17](=[O:18])[O:19][CH2:20][CH3:21])=[N:3]2

참가 물질

5

반응물 3

HCID 1049PyridineHCID 10928Ethyl chloroformateHCID 692404792-Amino-6,7-difluoro-3-methoxyquinoxaline

생성물 1

HCID 69244192Ethyl N-(6,7-difluoro-2-methoxyquinoxalin-3-yl)carbamate수율 60%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Amino-6,7-di fluoro-3-methoxyquinoxaline (550 mg, 2.60 mmol) and ethyl chloroformate (564 mg, 5.20 mmol) were dissolved in dichloromethane (50 ml) at room temperature and thereto pyridine (411 mg, 5.20 mmol) was added. The mixture was stirred at room temperature for 13 hours and concentrated under the reduced pressure to remove the solvent, and purified by SiO2 column chromatography. Extraction of the residue with a n-hexane:ethyl acetate (3:1) mixture and concentration gave 440 mg of the titled compound (yield, 60%).

후처리

  1. concentrationconcentrated under the reduced pressure
  2. customto remove the solvent
  3. custompurified by SiO2 column chromatography
  4. extractionExtraction of the residue
  5. concentrationwith a n-hexane:ethyl acetate (3:1) mixture and concentration

출처 및 근거

ORD 기록
ord-509dbdddee3943ba83f309a6e17277ac
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314100B2

연결된 노트

불러오는 중…