反应详情

Into a 100 ml reaction flask equipped with thermometer, reflux condenser and magnetic stirring bar and hot plate with magnetic stirring apparatus is placed 0.5 grams of para-toluenesulfonic acid, 5.0 ml cyclohexane and 6.1 grams (0.05 moles) of 2,3-butanedithiol. Over a period of 25 minutes, 5.3 grams (0.05 moles) of benzaldehyde is added to the reaction mass with stirring. The reaction mass is then heated to reflux with stirring and refluxed for a period of 9.5 hours while taking off water of reaction. At the end of 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 aqueous sodium chloride solution, dried over anhydrous sodium sulfate and filtered. The resulting filtrate is distilled on a Microvigreux column yielding the following three fractions:

1. customInto a 100 ml reaction flask
2. customequipped with thermometer
3. temperaturereflux condenser and magnetic stirring bar
4. temperatureThe reaction mass is then heated
5. temperatureto reflux
6. stirringwith stirring
7. temperaturerefluxed for a period of 9.5 hours
8. customtransferred to a separatory funnel
9. washThe reaction mass is then washed with one 50 ml portion of saturated aqueous sodium chloride solution
10. dry with materialdried over anhydrous sodium sulfate
11. filtrationfiltered
12. distillationThe resulting filtrate is distilled on a Microvigreux column
13. customyielding the following three fractions