反応 #62700

反応方程式

Hydrogen peroxide

n-octylmercaptan

Alpha-pinene

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

→

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

溶媒

Isopropanol

反応条件

後処理

1. 1
   温度The reaction was maintained at 155° C. for 15 min.
2. 2
   温度cooled
3. 3
   温度while maintaining the temperature at 40°-50° C
4. 4
   抽出The product was extracted with 150 ml of n-hexane
5. 5
   洗浄washed with 150 ml of 1M sodium carbonate
6. 6
   乾燥The organic layer was dried over magnesium sulfate
7. 7
   ろ過filtered
8. 8
   その他the solvent removed by rotary evaporation

実験手順

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.

出典