反应详情

Into a 100 ml reaction flask equipped with spin bar, reflux condenser, heating mantle, hot plate apparatus (with magnetic stirring apparatus) is placed 5 ml cyclohexane, 0.2 grams paratoluenesulfonic acid and 5.3 grams (0.05 moles) of 3-mercapto-2-butanol. Over a period of 30 minutes, 5.2 grams (0.05 moles) of 3-methylthiopropionaldehyde are added to the reaction mass. The reaction mass is then heated to reflux and water of reaction is continuously removed during the refluxing of the reaction mass. The reaction takes place over a period of 7 hours. At the end of the 7 hours the reaction mass is transferred to a separatory funnel and the reaction mass is washed with one 50 ml portion of saturated aqueous sodium chloride solution and then dried over anhydrous sodium sulfate. The product is then 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 continuously removed during the
8. temperaturerefluxing of the reaction mass
9. customof 7 hours
10. customAt the end of the 7 hours the reaction mass is transferred to a separatory funnel
11. washthe reaction mass is washed with one 50 ml portion of saturated aqueous sodium chloride solution
12. dry with materialdried over anhydrous sodium sulfate
13. filtrationThe product is then filtered
14. distillationdistilled on a Microvigreux column
15. customyielding the following fractions