Sodium hydrosulfide → HCID 178418602, Verbindung

HRID 5816

Reaktionsgleichung

Reaktionsgleichung von HRID 5816
Cl[C:2]1[CH:11]=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[SH-:12].[Na+]>CN(C)C=O>[SH:12][C:2]1[CH:11]=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1

Komponenten

4

Edukt 2

HCID 28015Sodium hydrosulfideHCID 2389382-Chloroquinoxaline

Produkt 1

HCID 178418602HCID 178418602, VerbindungAusbeute 157,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

2-Chloroquinoxaline (2 g) and sodium hydrosulphide (1.23 g) were stirred together in 25 ml of dimethylformamide and heated to 100° C. After 3 hours the reaction mixture was allowed to cool and then partitioned between 70 ml of water and 30 ml of ethyl acetate. The organic layer was separated and the aqueous layer extracted twice with 20 ml of ethyl acetate. The combined organic extracts were washed with sodium chloride solution, dried over anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure to yield an orange solid (3.1 g). The product of this reaction was used in the next preparative step without further purification.

Aufarbeitung

  1. temperatureto cool
  2. custompartitioned between 70 ml of water and 30 ml of ethyl acetate
  3. customThe organic layer was separated
  4. extractionthe aqueous layer extracted twice with 20 ml of ethyl acetate
  5. washThe combined organic extracts were washed with sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customthe solvent removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-774ce888c2ae4a3eb24f6b6510e760c5
Quelldatensatz
uspto-grants-1993_09
Patentnummer
US05246933

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