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Pyridine → Ethyl N-(6-fluoro-2-methoxyquinoxalin-3-yl)carbamate

HRID 1907443
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반응식

HRID 1907443 반응식
[NH2:1][C:2]1[C:3]([O:13][CH3:14])=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][C:8]([F:12])=[CH:7][CH:6]=2.Cl[C:16]([O:18][CH2:19][CH3:20])=[O:17].N1C=CC=CC=1>ClCCl>[F:12][C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][CH:7]=1)[N:4]=[C:3]([O:13][CH3:14])[C:2]([NH:1][C:16](=[O:17])[O:18][CH2:19][CH3:20])=[N:11]2
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 10928Ethyl chloroformateHCID 669182127-Fluoro-3-methoxyquinoxalin-2-amine

생성물 1

HCID 66917965Ethyl N-(6-fluoro-2-methoxyquinoxalin-3-yl)carbamate수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Amino-6-fluoro-2-methoxyquinoxaline (580 mg, 3.00 mmol) and ethyl chloroformate (391 mg, 3.60 mmol) were dissolved in dichloromethane (50 ml) at room temperature and thereto pyridine (285 mg, 3.60 mmol) was added. The mixture was stirred at room temperature for 10 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 740 mg of the titled compound (yield, 93%).

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-8bcef14c8be044678df722ddea81096a
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598173B2

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