反応 #62702

反応方程式

water

t-butanol

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

alpha-pinene

→

final product

2-(2-Pinanylthio)-5-(t-butylthio)-1,3,4-thiadiazole

溶媒

Xylene

xylene

反応条件

後処理

1. 1
   その他(exothermic reaction)
2. 2
   温度The reaction was maintained at 135°-155° C. for 15 min
3. 3
   その他The reaction was fitted with a Dean Stark trap
4. 4
   その他The reaction was fitted with an addition funnel
5. 5
   温度refluxing
6. 6
   その他the water removal
7. 7
   その他were collected
8. 8
   その他Solvent was stripped by rotary evaporation
9. 9
   workup.ADDITIONThe product was mixed with calcium hydroxide (1 g), hexane (about 100 ml), and sufficient acetone (about 50 ml)
10. 10
    温度to maintain one liquid layer
11. 11
    ろ過The product was filtered
12. 12
    その他the solvent removed by rotary evaporation

実験手順

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.

出典