반응 #215584

반응 방정식

2,3-Dicyano-6-n-propylamino-6-chloropyrazine

benzylthiol

pyridine

water

→

2,3-dicyano-5-n-propylamino-6-(benzylthio)pyrazine

수율 30.4%

용매

acetone

반응 조건

후처리

1. 1
   온도The solution was cooled to 0° to 5° C
2. 2
   workup.ADDITIONwas added dropwise over the period of 30 minutes
3. 3
   workup.STIRRINGThe mixture was further stirred at 20° to 30° C. for 1 hour
4. 4
   농축concentrated under reduced pressure
5. 5
   기타to remove acetone
6. 6
   추출The residue was extracted with 100 ml of chloform
7. 7
   세척The extract was washed twice with 50 ml of water
8. 8
   건조dried over anhydrous calcium chloride
9. 9
   농축concentrated under reduced pressure
10. 10
    기타to afford a yellowish solid
11. 11
    기타Recrystallization of the solid from ethanol

실험 절차

2,3-Dicyano-6-n-propylamino-6-chloropyrazine (1.11 g; 0.005 mole) and 0.87 g (0.007 mole) of benzylthiol were dissolved in 50 ml of acetone. The solution was cooled to 0° to 5° C. With stirring, a solution prepared from 0.40 g (0.005 mole) of pyridine and 20 ml of water was added dropwise over the period of 30 minutes. The mixture was further stirred at 20° to 30° C. for 1 hour, and concentrated under reduced pressure to remove acetone. The residue was extracted with 100 ml of chloform. The extract was washed twice with 50 ml of water, dried over anhydrous calcium chloride, and concentrated under reduced pressure to afford a yellowish solid. Recrystallization of the solid from ethanol afforded 0.47 g (yield 30%) of 2,3-dicyano-5-n-propylamino-6-(benzylthio)pyrazine.

출처