反应详情

温度

140 °C

2,5-Dimercapto-1,3,4-thiadiazole (35 g, 0.23 mol) and alpha-pinene (35 g, 0.26 mol) were charged to a reaction vessel and heated cautiously to 140° C. (exothermic reaction). The reaction was maintained at 135°-155° C. for 15 min. The reaction was fitted with a Dean Stark trap filled with xylene. Xylene (15 ml) was charged to the reaction. The reaction was fitted with an addition funnel containing t-butanol (25 g, 0.34 mol). The alcohol was added slowly with the reaction refluxing. Sulfuric acid (3 drops) was added to accelerate the water removal. The reaction product was isolated after approximately 5 ml (about 0.25 mol) of water were collected. Solvent was stripped by rotary evaporation. The product was mixed with calcium hydroxide (1 g), hexane (about 100 ml), and sufficient acetone (about 50 ml) to maintain one liquid layer. The product was filtered using a filter aid and the solvent removed by rotary evaporation. This afforded the final product.

1. custom(exothermic reaction)
2. temperatureThe reaction was maintained at 135°-155° C. for 15 min
3. customThe reaction was fitted with a Dean Stark trap
4. customThe reaction was fitted with an addition funnel
5. temperaturerefluxing
6. customthe water removal
7. customwere collected
8. customSolvent was stripped by rotary evaporation
9. additionThe product was mixed with calcium hydroxide (1 g), hexane (about 100 ml), and sufficient acetone (about 50 ml)
10. temperatureto maintain one liquid layer
11. filtrationThe product was filtered
12. customthe solvent removed by rotary evaporation