Reaktion #549752

Reaktionsgleichung

3-methylthiopropionaldehyde

para-toluenesulfonic acid

cyclohexane

1,3-butanediol

→

4-METHYL-2-[2-(METHYLTHIO)ETHYL]-m-DIOXANE

Lösungsmittel

water

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
   workup.ADDITIONSlowly added to the reaction mass over a period of 30 minutes
6. 6
   TemperaturThe reaction mass is then heated
7. 7
   Temperaturto reflux
8. 8
   Temperaturrefluxed for a period of 9 hours
9. 9
   Sonstigeis removed from the reaction mass
10. 10
    TemperaturAt the end of the 9 hour refluxing period
11. 11
    Temperaturthe reaction mass is then cooled
12. 12
    Sonstigetransferred to a separatory funnel
13. 13
    Waschenwashed with one 50 ml portion of saturated sodium chloride solution
14. 14
    Trocknendried over anhydrous sodium sulfate
15. 15
    Filtrationfiltered
16. 16
    workup.DISTILLATIONdistilled on a Microvigreux column
17. 17
    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 0.2 grams para-toluenesulfonic acid, 5 ml cyclohexane and 4.5 grams of 1,3-butanediol. Slowly added to the reaction mass over a period of 30 minutes is 3-methylthiopropionaldehyde (5.2 grams; 0.05 moles). The reaction mass is then heated to reflux and refluxed for a period of 9 hours. During the refluxing process, water of reaction is removed from the reaction mass. At the end of the 9 hour refluxing period, the reaction mass is then cooled and transferred to a separatory funnel and washed with one 50 ml portion of saturated sodium chloride solution and then dried over anhydrous sodium sulfate, filtered and distilled on a Microvigreux column yielding the following fractions:

Quelle