HCID 178524392, compound → Picolinic acid

HRID 1941063Notes

Reaction equation

HRID 1941063 reaction equation
O[C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][CH:3]=1>O>[N:7]1[CH:2]=[CH:3][CH:4]=[CH:5][C:6]=1[C:8]([OH:10])=[O:9]

Participants

3

Reactant 1

HCID 178524392HCID 178524392, compound

Product 1

HCID 1018Picolinic acid

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

For isolation, the cell-free picolinic acid solution was precipitated with CaCl2 /H2SO4. For this purpose, the cell-free picolinic acid solution from Example 2 was diluted 3-fold and, while stirring, 0.5 equivalent of CaCl2 per equivalent of picolinic acid was added after the cell-free fermentation solution had been heated to 90° C. The resulting calcium/picolinic acid complex precipitated immediately. The resulting complex was cooled to 4° C. with stirring, filtered off on a glass flit (porosity 3) and washed with demineralized water. The filter cake was suspended in demineralized water and acidified to a pH of 2.5 with concentrated sulfuric acid. During this operation, the picolinic acid was dissolved out of the complex and, at the same time, insoluble calcium sulfate was formed. Since the free picolinic acid is very soluble in water it was possible to remove calcium sulfate by filtration. The picolinic acid solution was evaporated to dryness and analyzed. The crude yield was about 70 percent with a purity of 86 percent by titration. The water content was 0.7 percent measured by the Karl-Fischer method.

Workup

  1. customto remove calcium sulfate
  2. filtrationby filtration
  3. customThe picolinic acid solution was evaporated to dryness

Sources & evidence

ORD record
ord-b52183940c9b4edc9766f0353fc093d8
Source dataset
uspto-grants-1997_12
Patent number
US05702930

Reaction notes

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