Perchloric Acid → Bis (piperazine) p-dihydroxy benzene disulfonate

HRID 259524

Reaktionsgleichung

Reaktionsgleichung von HRID 259524
Cl(O)(=O)(=O)=O.O.O.O.O.O.O.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.Cl(O)(=O)(=O)=O.[NH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.[K+].[OH:30][C:31]1([S:42]([O-:45])(=[O:44])=[O:43])[CH:36]=[CH:35][C:34]([OH:37])=[CH:33][CH:32]1[S:38]([O-:41])(=[O:40])=[O:39].[K+].Cl([O-])(=O)(=O)=O.[K+]>O>[OH:30][C:31]1([S:42]([OH:45])(=[O:44])=[O:43])[CH:36]=[CH:35][C:34]([OH:37])=[CH:33][CH:32]1[S:38]([OH:41])(=[O:40])=[O:39].[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.[NH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1

Komponenten

7

Edukt 5

HCID 24247Perchloric AcidHCID 120181Piperazine, hexahydrate2×HCID 516900Potassium PerchlorateHCID 85529587Piperazine perchlorateHCID 131710108p-Dihydroxy benzene disulfonic acid potassium salt

Produkt 1

HCID 21151652Bis (piperazine) p-dihydroxy benzene disulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

To an aqueous solution of perchloric acid, containing 200 g of said acid in 500 ml of water 40 % solution), the amount of aqueous solution of piperazine hexahydrate required for neutralization is added. The required amount of piperazine hexahydrate is 388.46 g (C4H10N2.6H2O) dissolved in 500 ml of water. Preferably the pH of the neutralizing solution is controlled to a pH close to 6. The piperazine perchlorate solution is mixed with the warm solution of p-dihydroxy benzene disulfonic acid potassium salt, and is stirred until a copious precipitate of potassium perchlorate is formed, which then increases when the solution is left to cool for several hours. After filtering off the potassium perchlorate, the solution of piperazine p-dihydroxy benzene disulfonate is concentrated in a rotary evaporator, under vacuum, at 60° C., until crystals begin to form, and it is then left in a refrigerator. The product is filtered and recrystallized in water to give 388 g of bis (piperazine) p-dihydroxy benzene disulfonate, having a melting point of 270° C.

Aufarbeitung

  1. additionis added
  2. customa pH close to 6
  3. customis formed
  4. temperaturewhich then increases when the solution
  5. waitis left
  6. temperatureto cool for several hours
  7. filtrationAfter filtering off the potassium perchlorate
  8. concentrationthe solution of piperazine p-dihydroxy benzene disulfonate is concentrated in a rotary evaporator, under vacuum, at 60° C., until crystals
  9. customto form
  10. waitit is then left in a refrigerator
  11. filtrationThe product is filtered
  12. customrecrystallized in water

Quellen und Nachweise

ORD-Eintrag
ord-1db5aff696834dd39bde7175de86d98f
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04038390

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