反应详情

Into a 100 ml reaction flask equipped with spin bar, reflux condenser, heating mantle and hot plate with magnetic stirring apparatus is placed 5 ml cyclohexane, 0.2 grams para-toluenesulfonic acid and 3.1 grams (0.05 moles) of 1,2-ethanediol. Over a period of 30 minutes, 5.2 grams (0.05 moles) of 3-methylthiopropionaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and during reflux, water of formation is removed. The refluxing continues for a period of 9 hours. At the end of the 9 hour period, the reaction mass is cooled and transferred to a separatory funnel and washed with one 50 ml portion of saturated sodium chloride solution. The reaction mass is then dried over anhydrous sodium sulfate, filtered and distilled on a Microvigreux column yielding the following fractions:

1. customInto a 100 ml reaction flask
2. customequipped with spin bar
3. temperaturereflux condenser
4. temperatureheating mantle
5. temperatureThe reaction mass is then heated
6. temperatureto reflux
7. temperatureduring reflux
8. customwater of formation is removed
9. waitThe refluxing continues for a period of 9 hours
10. temperatureAt the end of the 9 hour period, the reaction mass is cooled
11. customtransferred to a separatory funnel
12. washwashed with one 50 ml portion of saturated sodium chloride solution
13. dry with materialThe reaction mass is then dried over anhydrous sodium sulfate
14. filtrationfiltered
15. distillationdistilled on a Microvigreux column
16. customyielding the following fractions