反应详情

Into a 100 cc reaction flask equipped with reflux condenser, magnetic stirring bar and thermometer and hot plate equipped with magnetic stirring apparatus is placed 5 ml cyclohexane, 0.2 grams of para-toluenesulfonic acid and 5.4 grams (0.05 moles) of 1,2-propanedithiol. With stirring, over a period of 30 minutes, 6 grams (0.05 moles) of phenylacetaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and refluxed for a period of 8 hours. During the refluxing period, water of reaction is removed. At the end of the refluxing period, the reaction mass is cooled to room temperature and transferred to a separatory funnel. The reaction mass is then washed with one 50 ml portion of saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and filtered. The resulting filtrate is distilled on a Microvigreux column yielding the following three fractions:

1. customInto a 100 cc reaction flask
2. customequipped
3. temperaturewith reflux condenser, magnetic stirring bar
4. customthermometer and hot plate equipped with magnetic stirring apparatus
5. temperatureThe reaction mass is then heated
6. temperatureto reflux
7. temperaturerefluxed for a period of 8 hours
8. customis removed
9. customtransferred to a separatory funnel
10. washThe reaction mass is then washed with one 50 ml portion of saturated aqueous sodium chloride solution
11. dry with materialdried over anhydrous sodium sulfate
12. filtrationfiltered
13. distillationThe resulting filtrate is distilled on a Microvigreux column
14. customyielding the following three fractions