Acetic Acid → HCID 178429417, compound

HRID 236801Notes

Reaction equation

HRID 236801 reaction equation
[K].[CH:2]([C:4]1[C:5]([OH:12])=[N:6][C:7]([OH:11])=[CH:8][C:9]=1[CH3:10])=[O:3].[K].C(O)(=O)C>O>[CH:2]([C:4]1[C:5]([OH:12])=[N:6][C:7]([OH:11])=[CH:8][C:9]=1[CH3:10])=[O:3]

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 5462222PotassiumHCID 178429418HCID 178429418, compound

Product 1

HCID 178429417HCID 178429417, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The conversion of the potassium salt into the metal-free compound is carried out as follows: 19.1 parts of the crude product obtained in Example 2 are suspended in 200 parts of a mixture of 160 parts of acetic acid and 40 parts of water, and the reaction mixture is concentrated to 50 parts under vacuum, with warming. On allowing the concentrated solution to stand, the metal-free compound crystallizes out and is filtered off. The pure 3-formyl-4-methyl-2,6-dihydroxy pyridine, with a melting point of 180°-182° C., is obtained by redissolution and recrystallization from a mixture of 160 parts of ethanol and 40 parts of water.

Workup

  1. concentrationthe reaction mixture is concentrated to 50 parts under vacuum
  2. temperaturewith warming
  3. customthe metal-free compound crystallizes out and
  4. filtrationis filtered off

Sources & evidence

ORD record
ord-1f9fd4b2bef843a289b18bbfa52767c3
Source dataset
uspto-grants-1979_06
Patent number
US04157446

Reaction notes

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