HCID 178526554, compound → HCID 178507456, compound

HRID 2416089Notes

Reaction equation

HRID 2416089 reaction equation
[OH:1][C:2]1[C:11]([OH:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[N+:13]([O-])=O)[N:3]=1>CO.O1CCOCC1>[OH:1][C:2]1[C:11]([OH:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[NH2:13])[N:3]=1

Participants

3

Reactant 1

HCID 178526554HCID 178526554, compound

Product 1

HCID 178507456HCID 178507456, compound

Reagents, catalysts & solvents 1

HCID 21966525Dioxane MethanolSolvent

Procedure

2.00 g of 2,3-dihydroxy-5-nitroquinoxaline was dissolved in 1:1 mixed solvent of methanol/dioxane, then the reaction system was sufficiently flushed with argon, and 1.00 g of Pd/C (anhydrous) was added to the reaction mixture. Thereafter, the reaction system was flushed with hydrogen, and reaction was allowed at room temperature for 20 hr. After the reaction was over, the reaction mixture was dispersed in a solution of 6.00 g of potassium carbonate in 130 ml of water, thereby dissolving the reaction product. Filtration was conducted, and 35% hydrochloric acid was gradually added to the solution obtained upon the filtration, to obtain precipitates.

Workup

  1. customthe reaction system was sufficiently flushed with argon, and 1.00 g of Pd/C (anhydrous)
  2. additionwas added to the reaction mixture
  3. customThereafter, the reaction system was flushed with hydrogen, and reaction
  4. additionwas dispersed in a solution of 6.00 g of potassium carbonate in 130 ml of water
  5. dissolutiondissolving the reaction product
  6. filtrationFiltration
  7. addition35% hydrochloric acid was gradually added to the solution
  8. customobtained upon the filtration
  9. customto obtain
  10. customprecipitates

Sources & evidence

ORD record
ord-f506df5ad5234c56ad627f3f373b6373
Source dataset
uspto-grants-2004_11
Patent number
US06822069B2

Reaction notes

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