Reaktion #5912

Reaktionsgleichung

2-Chloroquinoxaline

sodium hydrosulphide

→

solid

Ausbeute 157.3%

2-mercaptoquinoxaline

Ausbeute 157.3%

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto cool
2. 2
   Sonstigepartitioned between 70 ml of water and 30 ml of ethyl acetate
3. 3
   SonstigeThe organic layer was separated
4. 4
   Extraktionthe aqueous layer extracted twice with 20 ml of ethyl acetate
5. 5
   WaschenThe combined organic extracts were washed with sodium chloride solution
6. 6
   Trocknendried over anhydrous magnesium sulphate
7. 7
   Filtrationfiltered
8. 8
   Sonstigethe solvent removed under reduced pressure

Vorschrift

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.

Quelle