Dimethyl Sulfoxide → HCID 22903580, 화합물

HRID 1488970

반응식

HRID 1488970 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 22903580HCID 22903580, 화합물수율 79.6%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-b1eda07ea62c4b62b01ad54716b65a27
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677305

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