Calcium Chloride → HCID 87972024, compound

HRID 489125Notes

Reaction equation

HRID 489125 reaction equation
[Na].[S:2]([C:6]1[CH:7]=[C:8]([C:16]([O:18][CH3:19])=[O:17])[CH:9]=[C:10]([CH:15]=1)[C:11]([O:13][CH3:14])=[O:12])([OH:5])(=[O:4])=[O:3].[Na].[Cl-].[Ca+2:22].[Cl-]>O>[Ca:22].[S:2]([C:6]1[CH:15]=[C:10]([C:11]([O:13][CH3:14])=[O:12])[CH:9]=[C:8]([CH:7]=1)[C:16]([O:18][CH3:19])=[O:17])([OH:5])(=[O:4])=[O:3]

Participants

5

Reactant 3

HCID 5284359Calcium ChlorideHCID 5360545SodiumHCID 451574393965-55-7

Product 1

HCID 87972024HCID 87972024, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Conditions

Temperature
30 °C

Procedure

296 Grams of dimethyl 5-sulfoisophthalate sodium salt were placed together with 2000 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 900 g of ion exchanged water was then gradually added dropwise to the thus obtained solution. The resulting mixture was cooled to 30° C. and filtered to separate white precipitates. The precipitates were dispersed in 3000 g of ion exchanged water. The dispersion was heated to 80° C., maintained at that temperature for 1 hour, cooled to 30° 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 120° C. for 5 hours to obtain 156 g of dimethyl 5-sulfoisophthalate calcium salt (Compound of the above formula (2)) as a white powder. The atomic absorption analysis revealed that the 5-sulfoisophthalic acid calcium salt powder contained 6.8% 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. filtrationfiltered
  5. customto separate white precipitates
  6. additionThe precipitates were dispersed in 3000 g of ion
  7. temperatureThe dispersion was heated to 80° C.
  8. temperaturemaintained at that temperature for 1 hour
  9. temperaturecooled to 30° C.
  10. filtrationfiltered
  11. washThe precipitates were washed with water
  12. temperatureheating
  13. filtrationfiltration
  14. washwashing steps
  15. customThe thus obtained
  16. customprecipitates
  17. customwere dried at 120° C. for 5 hours

Sources & evidence

ORD record
ord-6f784444118243a391ee88ef90cf0167
Source dataset
uspto-grants-2005_12
Patent number
US06977129B2

Reaction notes

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