反応 #549752

反応方程式

3-methylthiopropionaldehyde

para-toluenesulfonic acid

cyclohexane

1,3-butanediol

→

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

溶媒

water

反応条件

後処理

1. 1
   その他Into a 100 ml reaction flask
2. 2
   その他equipped with spin bar
3. 3
   温度reflux condenser
4. 4
   温度heating mantle
5. 5
   workup.ADDITIONSlowly added to the reaction mass over a period of 30 minutes
6. 6
   温度The reaction mass is then heated
7. 7
   温度to reflux
8. 8
   温度refluxed for a period of 9 hours
9. 9
   その他is removed from the reaction mass
10. 10
    温度At the end of the 9 hour refluxing period
11. 11
    温度the reaction mass is then cooled
12. 12
    その他transferred to a separatory funnel
13. 13
    洗浄washed with one 50 ml portion of saturated sodium chloride solution
14. 14
    乾燥dried over anhydrous sodium sulfate
15. 15
    ろ過filtered
16. 16
    workup.DISTILLATIONdistilled on a Microvigreux column
17. 17
    その他yielding the following fractions

実験手順

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:

出典