반응 #62700

반응 방정식

Hydrogen peroxide

n-octylmercaptan

Alpha-pinene

2,5-dimercapto-1,3,4-thiadiazole

→

2-(2-Pinanylthio)-5-(octyldithio)-1,3,4-thiadiazole

용매

Isopropanol

반응 조건

후처리

1. 1
   온도The reaction was maintained at 155° C. for 15 min.
2. 2
   온도cooled
3. 3
   온도while maintaining the temperature at 40°-50° C
4. 4
   추출The product was extracted with 150 ml of n-hexane
5. 5
   세척washed with 150 ml of 1M sodium carbonate
6. 6
   건조The organic layer was dried over magnesium sulfate
7. 7
   여과filtered
8. 8
   기타the solvent removed by rotary evaporation

실험 절차

Alpha-pinene (38 g, 0.28 mol) and 2,5-dimercapto-1,3,4-thiadiazole (40 g, 0.27 mol) were charged to the reaction flask and cautiously heated to 155° C. since the reaction was exothermic. The reaction was maintained at 155° C. for 15 min. and then cooled. Isopropanol (32 g) and n-octylmercaptan (43.7 g, 0.30 mol) were charged. Hydrogen peroxide, 35% (60 g, 0.62 mol) was added slowly while maintaining the temperature at 40°-50° C. The reaction was then allowed to stand overnight. The product was extracted with 150 ml of n-hexane and washed with 150 ml of 1M sodium carbonate. The organic layer was dried over magnesium sulfate, filtered, and the solvent removed by rotary evaporation.

출처