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 3.8 grams (0.05 moles) of 1,2-propanediol. Over a period of 8 hours, 3-methylthiopropionaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and during refluxing water of formation is removed. The refluxing continues for a period of 7 hours. At the end of the 7 hour period, the reaction mass is transferred to a separatory funnel and washed with one 50 ml portion of saturated aqueous sodium chloride solution and 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. customis removed
8. waitThe refluxing continues for a period of 7 hours
9. customAt the end of the 7 hour period, the reaction mass is transferred to a separatory funnel
10. washwashed with one 50 ml portion of saturated aqueous sodium chloride solution
11. dry with materialdried over anhydrous sodium sulfate
12. filtrationfiltered
13. distillationdistilled on a Microvigreux column
14. customyielding the following fractions