Acetone → HCID 23697072, Verbindung

HRID 2068002Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2068002
S([O-])([O-])=O.[Na+:5].[Na+].CC(C)=O.[CH3:11][C:12]1[C:16]([S:17](Cl)(=[O:19])=[O:18])=[C:15]([CH3:21])[O:14][N:13]=1.C(=O)([O-])[O-].[Na+].[Na+]>O>[CH3:11][C:12]1[C:16]([S:17]([O-:19])=[O:18])=[C:15]([CH3:21])[O:14][N:13]=1.[Na+:5]

Komponenten

6

Edukt 4

HCID 180AcetoneHCID 10340Sodium CarbonateHCID 24437Sodium SulfiteHCID 27363193,5-Dimethylisoxazole-4-sulfonyl chloride

Produkt 1

HCID 23697072HCID 23697072, VerbindungAusbeute 101,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A solution of sodium sulfite (680 mg, 5.40 mmol) in water (5 mL) was added to an acetone (5 mL) solution of 3,5-dimethylisoxazole-4-sulfonyl chloride (530 mg, 2.70 mmol). The mixture was heated to 80° C., then a solution of sodium carbonate (430 mg, 4.05 mmol) in water (5 ml) was added dropwise. The mixture was refluxed for 16 hours then evaporated to dryness. The residue was refluxed with ethanol (20 mL), the inorganics were removed by filtration. Evaporation of the filtrate afforded 500 mg of crude sodium 3,5-dimethylisoxazole-4-sulfinate. It was used in the next steps without further purification. 1H NMR (400 MHz, DMSO-d6): δ 2.37 (s, 3H) and 2.22 (s, 3H).

Aufarbeitung

  1. temperatureThe mixture was refluxed for 16 hours
  2. customthen evaporated to dryness
  3. temperatureThe residue was refluxed with ethanol (20 mL)
  4. customthe inorganics were removed by filtration
  5. customEvaporation of the filtrate

Quellen und Nachweise

ORD-Eintrag
ord-16cc4349b324424487aa1cf4f126e3ad
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08293919B2

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