反应详情

温度

155 °C

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.

1. temperatureThe reaction was maintained at 155° C. for 15 min.
2. temperaturecooled
3. temperaturewhile maintaining the temperature at 40°-50° C
4. extractionThe product was extracted with 150 ml of n-hexane
5. washwashed with 150 ml of 1M sodium carbonate
6. dry with materialThe organic layer was dried over magnesium sulfate
7. filtrationfiltered
8. customthe solvent removed by rotary evaporation