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

HRID 1878299노트

반응식

HRID 1878299 반응식
[NH2:1][C:2]1[C:11]([O:12][CH3:13])=[N:10][C:9]2[C:4](=[CH:5][C:6]([O:16][CH3:17])=[C:7]([O:14][CH3:15])[CH:8]=2)[N:3]=1.Cl[C:19]([O:21][CH2:22][CH3:23])=[O:20].N1C=CC=CC=1>ClCCl>[CH3:13][O:12][C:11]1[C:2]([NH:1][C:19](=[O:20])[O:21][CH2:22][CH3:23])=[N:3][C:4]2[C:9](=[CH:8][C:7]([O:14][CH3:15])=[C:6]([O:16][CH3:17])[CH:5]=2)[N:10]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 10928Ethyl chloroformateHCID 692443442-Amino-3,6,7-trimethoxyquinoxaline

생성물 1

HCID 69244380Ethyl N-(2,6,7-trimethoxyquinoxalin-3-yl)carbamate수율 90%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Amino-3,6,7-trimethoxyquinoxaline (2.60 g, 11.0 mmol) and ethyl chloroformate (2.40 g, 22.1 mmol) were dissolved in dichloromethane (50 ml) at room temperature and thereto pyridine (1.75 g, 22.1 mmol) was added. The mixture was stirred at room temperature for 22 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 3.04 g of the titled compound (yield, 90%).

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-d403b6f8f8b64dae9acc1c6804f389db
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314100B2

반응 노트

불러오는 중…