Hydrochloric Acid → 1-Naphthalenesulfinic acid

HRID 465490Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 465490
C(=O)(O)[O-].[Na+].S([O-])([O-])=O.[Na+].[Na+].[C:12]1([S:22](Cl)(=[O:24])=[O:23])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[CH:14][CH:13]=1.Cl>O>[C:12]1([S:22]([OH:24])=[O:23])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[CH:14][CH:13]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 24437Sodium SulfiteHCID 665601-Naphthalenesulfonyl chlorideHCID 516892Sodium Bicarbonate

Produkt 1

HCID 108887691-Naphthalenesulfinic acidAusbeute 62,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a vigorously stirred solution of sodium bicarbonate (8.4 g, 100 mmol) and anhydrous sodium sulphite (12 g, 95 mmol) in water (50 ml) at 70°-80° C., was added naphthalene-1-sulphonyl chloride (11.5 g, 50 mmol) in portions and with vigorous stirring. The temperature was kept at 70°-80° C. by intermittent heating. When the addition was complete, the mixture was heated and stirred at 70°-80° C. for a further hour. The mixture was then allowed to cool to room temperature over 4 hours and acidified with 2M hydrochloric acid. The precipitated solid was collected by filtration, washed with water, air dried and then recrystallised from aqueous ethanol to give naphthalene-1-sulphinic acid as a solid (6.0 g), m.p. 86 87° C.

Aufarbeitung

  1. customwas kept at 70°-80° C. by intermittent heating
  2. additionWhen the addition
  3. temperaturethe mixture was heated
  4. filtrationThe precipitated solid was collected by filtration
  5. washwashed with water, air
  6. customdried
  7. customrecrystallised from aqueous ethanol

Quellen und Nachweise

ORD-Eintrag
ord-06d7c58b39304e26bb5fc049d63eb8c2
Quelldatensatz
uspto-grants-1992_10
Patentnummer
US05153227

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