Dimethyl Sulfoxide → HCID 22903580、化合物

HRID 1488970

反応式

HRID 1488970 の反応式
F[C:2]1[CH:11]=[C:10]2[C:5]([NH:6][C:7](=[O:13])[C:8](=[O:12])[NH:9]2)=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].[Cl:17][C:18]1[CH:19]=[N:20][CH:21]=[C:22]([Cl:25])[C:23]=1[OH:24].[OH-].[K+].CS(C)=O>CC(C)=O>[N+:14]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:2]=1[N:20]1[CH:21]=[C:22]([Cl:25])[C:23](=[O:24])[C:18]([Cl:17])=[CH:19]1)[NH:9][C:8](=[O:12])[C:7](=[O:13])[NH:6]2)([O-:16])=[O:15]

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 14797Potassium HydroxideHCID 99912306-Fluoro-7-nitro-1,4-dihydroquinoxaline-2,3-dioneHCID 178516337HCID 178516337、化合物

生成物 1

HCID 22903580HCID 22903580、化合物収率 79.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

First, 1.129 g of 7-fluoro-6-nitro-1,4-dihydroquinoxaline-2,3-dione, 1.648 g of 3,5-dichloro-4-hydroxypyridine, and 672 mg of powdered potassium hydroxide were added to 10 ml of dry dimethylsulfoxide. The mixture was allowed to react at 130° C. for 3 hours in a nitrogen atmosphere. The subsequent processes were conducted in the same way as in Example 2. The resultant precipitate was dissolved by heating in dimethylformaldehyde and the solution was decolorized with activated carbon and filtered. Water in an equal amount was added thereto and the solution was allowed to stand overnight to give 1.473 g of crystals of 6-nitro-7-(3,5-dichloro-4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione.

後処理

  1. customto react at 130° C. for 3 hours in a nitrogen atmosphere
  2. filtrationfiltered
  3. additionWater in an equal amount was added

出典と根拠

ORDレコード
ord-b1eda07ea62c4b62b01ad54716b65a27
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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