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 6.1 grams (0.05 moles) of 2,3-butanedithiol. Over a period of 30 minutes with stirring is added to the reaction mass 7.6 grams (0.05 moles) of citral having the structure: ##STR23## After the citral is added, the reaction mass is heated to reflux and refluxed (with removal of water of reaction) over a period of 9 hours. At the end of the 9 hour 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 and then dried over anhydrous sodium sulfate, 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 heated
6. temperatureto reflux
7. temperaturerefluxed
8. custom(with removal of water of reaction) over a period of 9 hours
9. temperatureAt the end of the 9 hour period, the reaction mass is cooled
10. customtransferred to a separatory funnel
11. washThe reaction mass is then washed with one 50 ml portion of saturated sodium chloride solution
12. dry with materialdried over anhydrous sodium sulfate
13. filtrationfiltered
14. distillationdistilled on a Microvigreux column
15. customyielding the following fractions