Sodium 4-cyanobenzenesulfinate → 3-Ethyl-2-methylbenzoxazolium 4-Cyanobenzenesulfinate

HRID 1796448Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1796448
[Cl-].[CH2:2]([N+:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]=1[CH3:13])[CH3:3].[C:14]([C:16]1[CH:21]=[CH:20][C:19]([S:22]([O-:24])=[O:23])=[CH:18][CH:17]=1)#[N:15].[Na+]>C(O)C>[C:14]([C:16]1[CH:17]=[CH:18][C:19]([S:22]([O-:24])=[O:23])=[CH:20][CH:21]=1)#[N:15].[CH2:2]([N+:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]=1[CH3:13])[CH3:3]

Komponenten

4

Edukt 2

HCID 23668300Sodium 4-cyanobenzenesulfinateHCID 67174878HCID 67174878, Verbindung

Produkt 1

HCID 220550573-Ethyl-2-methylbenzoxazolium 4-CyanobenzenesulfinateAusbeute 46,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

A solution of 3-ethyl-2-methylbenzoxazolium chloride (0.73 g) in ethanol (20 mL) was added to an Erlenmeyer flask containing a magnetically stirred boiling solution of sodium 4-cyanobenzenesulfinate (0.1 g) in anhydrous ethanol (20 mL). The mixture was allowed to cool to room temperature and was then further cooled in an ice bath. The mixture was filtered and the filtrate was concentrated to dryness using a rotary evaporator. The residue was mixed with deionized water and this mixture was extracted with ethyl acetate (2×20 mL). The combined organic extracts were concentrated to dryness using a rotary evaporator. The resultant solid was then dissolved in methylene chloride, filtered and evaporated to dryness using a rotary evaporator to afford 0.08 g of product.

Aufarbeitung

  1. additioncontaining
  2. temperaturewas then further cooled in an ice bath
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated to dryness
  5. customa rotary evaporator
  6. additionThe residue was mixed with deionized water
  7. extractionthis mixture was extracted with ethyl acetate (2×20 mL)
  8. concentrationThe combined organic extracts were concentrated to dryness
  9. customa rotary evaporator
  10. dissolutionThe resultant solid was then dissolved in methylene chloride
  11. filtrationfiltered
  12. customevaporated to dryness
  13. customa rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-8ec8363219d34379ac2d9558e0652a27
Quelldatensatz
uspto-grants-2006_04
Patentnummer
US07030169B2

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