Water → HCID 2826629, compound

HRID 569738Notes

Reaction equation

HRID 569738 reaction equation
[NH2:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][C:11]=1[NH2:12])[C:5]([O:7][CH3:8])=[O:6].O>C1(C)C=CC=CC=1>[CH3:3][C:2]1[C:11]([CH3:10])=[N:1][C:2]2[C:11](=[CH:10][CH:9]=[C:4]([C:5]([O:7][CH3:8])=[O:6])[CH:3]=2)[N:12]=1

Participants

4

Reactant 2

HCID 962WaterHCID 1355243,5-Diamino-2-methylbenzoic acid

Product 1

HCID 2826629HCID 2826629, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

55.8 g (0.354 mole) of methyl 3,4-diaminobenzoate and 30.5 g (0.354 mole) of diacetyl are heated under reflux in 500 ml of toluene for 3 hours, using a water separator. The toluene is distilled off in vacuo and the residue is dissolved in ethyl acetate under the influence of heat, active charcoal being added, the active charcoal is separated off via a Seitz filter and the filtrate is concentrated to dryness.

Workup

  1. distillationThe toluene is distilled off in vacuo
  2. dissolutionthe residue is dissolved in ethyl acetate under the influence
  3. temperatureof heat
  4. additionactive charcoal being added
  5. customthe active charcoal is separated off via a Seitz
  6. filtrationfilter
  7. concentrationthe filtrate is concentrated to dryness

Sources & evidence

ORD record
ord-fd91cf51dc7044edb27e31c6088f0903
Source dataset
uspto-grants-1988_03
Patent number
US04734407

Reaction notes

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