Sulfuric Acid → Methyl 3-chloro-7-methoxy-2-oxo-1,2-dihydroquinoxaline-6-carboxylate

HRID 1403589ノート

反応式

HRID 1403589 の反応式
[Cl:1][C:2]1[C:3](=[O:27])[N:4](CC2C=CC(OC)=CC=2)[C:5]2[C:10]([N:11]=1)=[CH:9][C:8]([C:12]([O:14][CH3:15])=[O:13])=[C:7]([O:16][CH3:17])[CH:6]=2.S(=O)(=O)(O)O>>[Cl:1][C:2]1[C:3](=[O:27])[NH:4][C:5]2[C:10]([N:11]=1)=[CH:9][C:8]([C:12]([O:14][CH3:15])=[O:13])=[C:7]([O:16][CH3:17])[CH:6]=2

参加物

3

反応物 2

HCID 1118Sulfuric AcidHCID 70664997Methyl 3-chloro-7-methoxy-1-(4-methoxybenzyl)-2-oxo-1,2-dihydroquinoxaline-6-carboxylate

生成物 1

HCID 70665121Methyl 3-chloro-7-methoxy-2-oxo-1,2-dihydroquinoxaline-6-carboxylate

実験手順

Methyl 3-chloro-7-methoxy-1-(4-methoxybenzyl)-2-oxo-1,2-dihydroquinoxaline-6-carboxylate (6.0 g, 15.43 mmol) was added to sulfuric acid (conc, 15 mL) in several batches with stirring at room temperature and then stirred for 10 minutes. The resulting solution was diluted with ice-water (100 mL) and extracted with ethyl acetate (3×200 mL). The organic layers were combined and dried over anhydrous magnesium sulfate and concentrated in vacuo to afford methyl 3-chloro-7-methoxy-2-oxo-1,2-dihydroquinoxaline-6-carboxylate as a yellow solid (2.5, 60%).

後処理

  1. stirringstirred for 10 minutes
  2. extractionextracted with ethyl acetate (3×200 mL)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-6b8f987a25734c15b1c1736f3f3a043e
出典データセット
uspto-grants-2014_12
特許番号
US08912188B2

反応ノート

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