Sodium Sulfite → Sodium 2-chlorobenzene-1-sulfinate

HRID 1944446Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1944446
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8](Cl)(=[O:10])=[O:9].O1CCOCC1.C(=O)(O)[O-].[Na+:22].S([O-])([O-])=O.[Na+].[Na+]>O>[Na+:22].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8]([O-:10])=[O:9]

Komponenten

6

Edukt 4

HCID 24437Sodium SulfiteHCID 312751,4-DioxaneHCID 761872-Chlorobenzenesulfonyl chlorideHCID 516892Sodium Bicarbonate

Produkt 1

HCID 23719078Sodium 2-chlorobenzene-1-sulfinateAusbeute 97,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

A mixture of 2-chlorobenzenesulfonyl chloride (2.5 g) and dioxane (35 mL) was treated with a mixture of sodium bicarbonate (2.0 g), sodium sulfite (3.0 g) and water (17 mL), and the resulting mixture was heated at 75° C. for 30 minutes. The mixture was cooled to room temperature and concentrated under reduced pressure. The residue was triturated with ethanol, filtered and the filtrate concentrated under reduced pressure. The residue was triturated with acetonitrile to afford the title compound as a white solid (2.3 g).

Aufarbeitung

  1. temperatureThe mixture was cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was triturated with ethanol
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated under reduced pressure
  6. customThe residue was triturated with acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-ce1e75f48d66433b9b338dc893c648cd
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08394836B2

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