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Sodium Hydroxide → Sodium m-mesyloxybenzenesulfinate

HRID 851540
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 851540
S([O-])([O-])=O.[Na+:5].[Na+].[S:7]([O:11][C:12]1[CH:13]=[C:14]([S:18](Cl)(=[O:20])=[O:19])[CH:15]=[CH:16][CH:17]=1)([CH3:10])(=[O:9])=[O:8].[OH-].[Na+]>O>[S:7]([O:11][C:12]1[CH:13]=[C:14]([S:18]([O-:20])=[O:19])[CH:15]=[CH:16][CH:17]=1)([CH3:10])(=[O:9])=[O:8].[Na+:5]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 13518302m-Mesyloxybenzenesulfonyl chloride

Produkt 1

HCID 23664830Sodium m-mesyloxybenzenesulfinate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of sodium sulfite (63 g; 0.5 mole) in water (400 ml) was added m-mesyloxybenzenesulfonyl chloride (67.7 g; 0.25 mole). The mixture was stirred vigorously, adding 50 percent sodium hydroxide solution as needed to maintain pH at 7 to 7.25, holding the temperature at 20° to 25° C. by means of a cold water bath. After 2 hours, a clear solution with a small amount of brown sludge was obtained. The mixture was filtered through Celite and the filtrate was poured into an evaporating dish and slowly allowed to evaporate. The first material to separate (32.5 g) was inorganic (by I. R. Spectrum). Further evaporation afforded three crops of crystalline material which was used without further purification.

Aufarbeitung

  1. temperatureto maintain pH at 7 to 7.25
  2. customat 20° to 25° C.
  3. customa clear solution with a small amount of brown sludge was obtained
  4. filtrationThe mixture was filtered through Celite
  5. additionthe filtrate was poured into an evaporating dish
  6. customto evaporate
  7. customThe first material to separate (32.5 g)
  8. customFurther evaporation
  9. customafforded three crops of crystalline material which
  10. customwas used without further purification

Quellen und Nachweise

ORD-Eintrag
ord-4610c700c61d4741a2ab538d49443110
Quelldatensatz
uspto-grants-1983_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04385104

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