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

HRID 1878275

反応式

HRID 1878275 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-509dbdddee3943ba83f309a6e17277ac
出典データセット
uspto-grants-2012_11
特許番号
US08314100B2

関連ノート

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