Acetic Acid → HCID 22507052, compound

HRID 1368851Notes

Reaction equation

HRID 1368851 reaction equation
[CH3:1][O:2][C:3]1[N:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([NH:11][C:12]2[CH:17]=[CH:16][C:15](C)=[CH:14][C:13]=2[N+:19]([O-])=O)[N:4]=1.[C:22](O)(=O)C>C(OCC)(=O)C.O.[Fe]>[CH3:10][O:9][C:7]1[N:8]=[C:3]([O:2][CH3:1])[N:4]=[C:5]([NH:11][C:12]2[C:13]([NH2:19])=[CH:14][CH:15]=[C:16]([CH3:22])[CH:17]=2)[N:6]=1

Participants

6

Reactant 2

HCID 176Acetic AcidHCID 22507060HCID 22507060, compound

Product 1

HCID 22507052HCID 22507052, compound

Reagents, catalysts & solvents 3

HCID 23925IronCatalystHCID 962WaterSolventHCID 8857Ethyl AcetateSolvent

Procedure

N-(4,6-dimethoxy-[1,3,5]triazin-2-yl)-4-methyl-2-nitroaniline (10 g) was dissolved in ethyl acetate (50 ml) and water (50 ml), and 10 g of iron power and acetic acid (2 ml) were added thereto, followed by reflux for 2 hours. Insoluble matters were removed by filtration, and the ethyl acetate layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous magnesium sulfate. The solvent was distilled off to obtain 8.8 g of the desired product as a white powder (m.p. 180-183° C.)

Workup

  1. temperatureby reflux for 2 hours
  2. customInsoluble matters were removed by filtration
  3. washthe ethyl acetate layer was washed with a saturated sodium chloride aqueous solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off

Sources & evidence

ORD record
ord-da5bfa52f3f44813a298523e8ab9d23d
Source dataset
uspto-grants-2003_06
Patent number
US06576631B1

Reaction notes

Loading…