Acetic Acid → HCID 19779931, compound

HRID 1533836Notes

Reaction equation

HRID 1533836 reaction equation
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[C:8]([N:12]2[CH:16]=[N:15][CH:14]=[N:13]2)[C:4]=1[C:5](N)=[O:6].C(O)(=[O:19])C>Cl>[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[C:8]([N:12]2[CH:16]=[N:15][CH:14]=[N:13]2)[C:4]=1[C:5]([OH:19])=[O:6]

Participants

4

Reactant 2

HCID 176Acetic AcidHCID 19779937HCID 19779937, compound

Product 1

HCID 19779931HCID 19779931, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

0.116 mol of the above crude 2-methoxy-6-(1,2,4-triazol-1-yl)-benzamide are stirred in a mixture of 120 ml of concentrated hydrochloric acid and 60 ml of glacial acetic acid for 5 h at 100° C. The mixture is evaporated down under reduced pressure and the process is repeated with the residue. After further evaporation of the mixture, the residue is dissolved in a little water and the solution is brought to pH 3 with sodium hydroxide solution. 30-40 ml of ethanol are added, after which the precipitate is filtered off under suction and dissolved in methanol. After the solution has been dried and evaporated down, 14.7 g of the above acid of melting point 200°-202° C. (decomposition) are isolated.

Workup

  1. customThe mixture is evaporated down under reduced pressure
  2. customAfter further evaporation of the mixture
  3. dissolutionthe residue is dissolved in a little water
  4. addition30-40 ml of ethanol are added
  5. filtrationafter which the precipitate is filtered off under suction
  6. dissolutiondissolved in methanol
  7. customAfter the solution has been dried
  8. customevaporated down

Sources & evidence

ORD record
ord-2d45016b9ba44408a21ad315f5625f58
Source dataset
uspto-grants-1992_02
Patent number
US05085686

Reaction notes

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