Oxalic Acid → HCID 23298023, compound

HRID 1953766Notes

Reaction equation

HRID 1953766 reaction equation
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([Cl:9])=[CH:4][C:3]=1[CH3:10].[C:11](O)(=[O:15])[C:12](O)=[O:13]>Cl.O>[Cl:9][C:5]1[CH:6]=[C:7]2[C:2]([NH:1][C:11](=[O:15])[C:12](=[O:13])[NH:8]2)=[C:3]([CH3:10])[CH:4]=1

Participants

5

Reactant 2

HCID 971Oxalic AcidHCID 15125155-Chloro-3-methylbenzene-1,2-diamine

Product 1

HCID 23298023HCID 23298023, compound

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolventHCID 962WaterSolvent

Procedure

123 g (0.79 mol) of 2,3-diamino-5-chlorotoluene and 106.2 g (1.18 mol) of oxalic acid are heated at reflux for 5 hours in 800 ml of 4N hydrochloric acid. The reaction mixture is allowed to cool, and is diluted with water, filtered off on a suction filter and washed with water. The product is then stirred in hot ethanol, filtered off on a suction filter and the suction filter material is dried in vacuo at 60°. The title compound is obtained as slightly grayish crystals of m.p.>250°.

Workup

  1. temperatureto cool
  2. filtrationfiltered off on a suction
  3. filtrationfilter
  4. washwashed with water
  5. filtrationfiltered off on a suction
  6. filtrationfilter
  7. filtrationthe suction filter material
  8. customis dried in vacuo at 60°

Sources & evidence

ORD record
ord-ce3b3127212e42208811feb46e3f6e8a
Source dataset
uspto-grants-2000_09
Patent number
US06117873

Reaction notes

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