Reaktion #549751

Reaktionsgleichung

para-toluenesulfonic acid

1,2-ethanediol

3-methylthiopropionaldehyde

→

2-[2-(METHYLTHIO)ETHYL]-1,3-DIOXOLANE

Lösungsmittel

cyclohexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeInto a 100 ml reaction flask
2. 2
   Sonstigeequipped with spin bar
3. 3
   Temperaturreflux condenser
4. 4
   Temperaturheating mantle
5. 5
   TemperaturThe reaction mass is then heated
6. 6
   Temperaturto reflux
7. 7
   Temperaturduring reflux
8. 8
   Sonstigewater of formation is removed
9. 9
   workup.WAITThe refluxing continues for a period of 9 hours
10. 10
    TemperaturAt the end of the 9 hour period, the reaction mass is cooled
11. 11
    Sonstigetransferred to a separatory funnel
12. 12
    Waschenwashed with one 50 ml portion of saturated sodium chloride solution
13. 13
    TrocknenThe reaction mass is then dried over anhydrous sodium sulfate
14. 14
    Filtrationfiltered
15. 15
    workup.DISTILLATIONdistilled on a Microvigreux column
16. 16
    Sonstigeyielding the following fractions

Vorschrift

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:

Quelle