Calcium Chloride → HCID 18755102, compound

HRID 489124Notes

Reaction equation

HRID 489124 reaction equation
[Na+].[S:2]([C:6]1[CH:7]=[C:8]([C:15]([O-:17])=[O:16])[CH:9]=[C:10]([CH:14]=1)[C:11]([O-:13])=[O:12])([OH:5])(=[O:4])=[O:3].[Na+].[Na].[Cl-].[Ca+2:21].[Cl-]>O>[Ca+2:21].[S:2]([C:6]1[CH:7]=[C:8]([C:15]([O-:17])=[O:16])[CH:9]=[C:10]([CH:14]=1)[C:11]([O-:13])=[O:12])([OH:5])(=[O:4])=[O:3]

Participants

5

Reactant 3

HCID 5284359Calcium ChlorideHCID 5360545SodiumHCID 21881961HCID 21881961, compound

Product 1

HCID 18755102HCID 18755102, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Conditions

Temperature
10 °C

Procedure

268 Grams of 5-sulfoisophthalic acid sodium salt were placed together with 500 g of ion exchanged water in a reactor equipped with a stirrer. The contents in the reactor were heated with stirring to 80° C. so that the sodium salt was dissolved in water. A solution of calcium chloride dissolved in an amount of 55.5 g into 100 g of ion exchanged water was then gradually added dropwise to the thus obtained solution. The resulting mixture was concentrated by evaporation to remove 250 g of water and then cooled to 10° C. and filtered to separate white precipitates. The precipitates were dispersed in 300 g of ion exchanged water. The dispersion was heated to 80° C., maintained at that temperature for 1 hour, cooled to 10° C. and then filtered. The precipitates were washed with water. Such a procedure including dispersion, heating, filtration and washing steps was repeated once more. The thus obtained precipitates were dried at 150° C. for 5 hours to obtain 141 g of 5-sulfoisophthalic acid calcium salt of the formula (3) shown below as a white powder. The atomic absorption analysis revealed that the 5-sulfoisophthalic acid calcium salt powder contained 7.5% by weight of calcium.

Workup

  1. customequipped with a stirrer
  2. temperatureThe contents in the reactor were heated
  3. additionwas then gradually added dropwise to the thus obtained solution
  4. concentrationThe resulting mixture was concentrated by evaporation
  5. customto remove 250 g of water
  6. filtrationfiltered
  7. customto separate white precipitates
  8. additionThe precipitates were dispersed in 300 g of ion
  9. temperatureThe dispersion was heated to 80° C.
  10. temperaturemaintained at that temperature for 1 hour
  11. temperaturecooled to 10° C.
  12. filtrationfiltered
  13. washThe precipitates were washed with water
  14. temperatureheating
  15. filtrationfiltration
  16. washwashing steps
  17. customThe thus obtained
  18. customprecipitates
  19. customwere dried at 150° C. for 5 hours

Sources & evidence

ORD record
ord-e2b7b7b6b88a40b4a1d1dfcd3b2cacdf
Source dataset
uspto-grants-2005_12
Patent number
US06977129B2

Reaction notes

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