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 0.5 grams para-toluenesulfonic acid, 5.0 ml cyclohexane and 5.4 grams (0.05 moles) of 1,2-propanedithiol. 7.6 grams (0.05 moles) of citral is then added to the reaction mass over a period of 30 minutes. After the addition of the citral, the reaction mass is heated to reflux and refluxed for a period of 10 hours while removing water of reaction. After the 10 hour reflux period, the reaction mass is cooled and transferred to a separatory funnel. The reaction mass is then washed with one 50 ml portion of saturated sodium chloride solution followed by drying over anhydrous sodium sulfate and filtration. The resulting filtrate is 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 heated
6. temperatureto reflux
7. temperaturerefluxed for a period of 10 hours
8. customwhile removing
9. customwater of reaction
10. temperatureAfter the 10 hour reflux period
11. temperaturethe reaction mass is cooled
12. customtransferred to a separatory funnel
13. washThe reaction mass is then washed with one 50 ml portion of saturated sodium chloride solution
14. dry with materialby drying over anhydrous sodium sulfate and filtration
15. distillationThe resulting filtrate is distilled on a Microvigreux column
16. customyielding the following fractions