反应详情

Into a 100 ml reaction flask equipped with magnetic stirring bar, thermometer and reflux condenser and hot plate with magnetic stirring apparatus is placed 0.5 grams para-toluenesulfonic acid, 5 ml cyclohexane and 6.1 grams (0.05 moles) of 2,3-butanedithiol. Over a period of 35 minutes, 4.8 grams (0.05 moles) of 2-furaldehyde is added to the reaction mass with stirring. The reaction mass is then heated to reflux and refluxed for a period of 7.5 hours with stirring while removing water to reaction. After the refluxing period, the reaction mass is cooled to room temperature and transferred to a separatory funnel. The reaction mass is then washed with one 50 ml portion of saturated sodium chloride soution and dried over anhydrous sodium sulfate and filtered. The resulting filtrate is distilled using a Microvigreux column yielding the following fractions:

1. customInto a 100 ml reaction flask
2. customequipped with magnetic stirring bar
3. temperaturethermometer and reflux condenser
4. temperatureThe reaction mass is then heated
5. temperatureto reflux
6. temperaturerefluxed for a period of 7.5 hours
7. stirringwith stirring
8. customwhile removing water
9. customto reaction
10. customtransferred to a separatory funnel
11. washThe reaction mass is then washed with one 50 ml portion of saturated sodium chloride soution
12. dry with materialdried over anhydrous sodium sulfate
13. filtrationfiltered
14. distillationThe resulting filtrate is distilled
15. customyielding the following fractions