2,6-Dihydroxybenzoic Acid → HCID 178524829, compound

HRID 1684420Notes

Reaction equation

HRID 1684420 reaction equation
[C:1]([OH:11])(=[O:10])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][C:8]=1[OH:9])[OH:4].[Bi]=O.[Bi:14]>O>[C:1]([O-:11])(=[O:10])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][C:8]=1[OH:9])[OH:4].[Bi+3:14].[C:1]([O-:11])(=[O:10])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][C:8]=1[OH:9])[OH:4].[C:1]([O-:11])(=[O:10])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][C:8]=1[OH:9])[OH:4]

Participants

5

Reactant 3

HCID 93382,6-Dihydroxybenzoic AcidHCID 5359367BismuthHCID 6327914Bismuth-oxygen

Product 1

HCID 178524829HCID 178524829, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
50 °C

Procedure

A 3-liter thermostatic reactor fitted with a pneumatic stirrer, a bottom valve, temperature probes, a reflux condenser and a heating system is employed for this synthesis. 900 ml of distilled water and 15.4 g of γ-resorcylic acid, that is 0.1 mole of acid, are placed in the reactor. The heterogeneous mixture is heated to 50° C. with stirring and then 31 g of bismuth oxide, that is 0.1 gram-atom of bismuth, are added portionwise over approximately 15 minutes. The suspension thus obtained is heated to 80° C. After approximately 30 minutes approximately 1500 ml of distilled water are added to permit better stirring of the suspension and the suspension is then left stirred for approximately 5 hours at 80° C. The mixture is then filtered hot and the cake obtained is then washed with 500 ml of ethanol. The product is next vacuum-dried at 60° C. over calcium chloride. At the end of reaction 24 g of bismuth γ-resorcylate are recovered.

Workup

  1. customA 3-liter thermostatic reactor fitted with a pneumatic stirrer, a bottom valve
  2. customtemperature probes, a reflux condenser and a heating system is employed for this synthesis
  3. additionare added portionwise over approximately 15 minutes
  4. customThe suspension thus obtained
  5. temperatureis heated to 80° C
  6. stirringto permit better stirring of the suspension
  7. waitthe suspension is then left
  8. stirringstirred for approximately 5 hours at 80° C
  9. filtrationThe mixture is then filtered hot
  10. customthe cake obtained
  11. washis then washed with 500 ml of ethanol
  12. dry with materialThe product is next vacuum-dried at 60° C. over calcium chloride
  13. customAt the end of reaction 24 g of bismuth γ-resorcylate
  14. customare recovered

Sources & evidence

ORD record
ord-220e378ae445415fbcba46d6be2aa361
Source dataset
uspto-grants-1997_06
Patent number
US05639987

Reaction notes

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