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

HRID 1878283

반응식

HRID 1878283 반응식
[NH2:1][C:2]1[C:11]([O:12][CH3:13])=[N:10][C:9]2[C:4](=[CH:5][C:6]([Cl:15])=[C:7]([Cl:14])[CH:8]=2)[N:3]=1.Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18].N1C=CC=CC=1>ClCCl>[Cl:15][C:6]1[CH:5]=[C:4]2[C:9](=[CH:8][C:7]=1[Cl: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 692433492-Amino-6,7-dichloro-3-methoxyquinoxaline

생성물 1

HCID 69243293Ethyl N-(6,7-dichloro-2-methoxyquinoxalin-3-yl)carbamate수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Amino-6,7-dichloro-3-methoxyquinoxaline (1.16 g, 4.75 mmol) and ethyl chloroformate (1.03 g, 9.50 mmol) were dissolved in dichloromethane (50 ml) at room temperature and thereto pyridine (751 mg, 9.50 mmol) was added. The mixture was stirred at room temperature for 24 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 (2:1) mixture and concentration gave 1.29 g of the titled compound (yield, 86%).

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 (2:1) mixture and concentration

출처 및 근거

ORD 기록
ord-882ee2faa6a347c5b2f867c1bbfcd2cb
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314100B2

연결된 노트

불러오는 중…