Sulfuric Acid → 6-nitro-7-(4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione

HRID 1488978

反応式

HRID 1488978 の反応式
[O:1]=[C:2]1[CH:7]=[CH:6][N:5]([C:8]2[CH:9]=[C:10]3[C:15](=[CH:16][CH:17]=2)[NH:14][C:13](=[O:18])[C:12](=[O:19])[NH:11]3)[CH:4]=[CH:3]1.S(=O)(=O)(O)O.[N+:25]([O-])([O-:27])=[O:26].[K+].[OH-].[Na+]>>[N+:25]([C:17]1[CH:16]=[C:15]2[C:10](=[CH:9][C:8]=1[N:5]1[CH:6]=[CH:7][C:2](=[O:1])[CH:3]=[CH:4]1)[NH:11][C:12](=[O:19])[C:13](=[O:18])[NH:14]2)([O-:27])=[O:26]

参加物

5

反応物 4

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 24434Potassium NitrateHCID 229035916-(4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione

生成物 1

HCID 98611296-nitro-7-(4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione収率 71%

反応条件

温度
60 °C

実験手順

First, 510 mg of 6-(4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione was added to 5 ml of conc. sulfuric acid with ice-cooling and dissolved therein. Then, 253 mg of potassium nitrate was added to the resultant solution. The mixture was heated at 60° C. for 3 hours with stirring. Then, 20 ml of ice water was added to the mixture and the pH of the solution was adjusted to 5 with a solution of 4N sodium hydroxide. The precipitated yellow crystals were filtered. The crystals thus obtained were washed with water and dried to give 426 mg of 6-nitro-7-(4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione.

後処理

  1. temperaturecooling
  2. dissolutiondissolved
  3. filtrationThe precipitated yellow crystals were filtered
  4. customThe crystals thus obtained
  5. washwere washed with water
  6. customdried

出典と根拠

ORDレコード
ord-eac2687ccd3248ef85b22d326c258b3c
出典データセット
uspto-grants-1997_10
特許番号
US05677305

関連ノート

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