反应详情

To a 2000 ml four-necked reaction flask, equipped with a magnetic stirrer, thermometer, addition funnel, condenser and a nitrogen sweep, was added 281 grams of thionyl chloride (2.38 moles), 1 ml of dimethyl formamide, and 1000 ml of toluene. 356 grams of the allyloxybenzoic acid (2.0 moles) as prepared above was added over approximately 20 minutes. The reaction temperature was kept below 20° C. with an ice/water bath. The nitrogen sweep was connected to a trap, which contained 1000 ml of a 4 M aq. NaOH solution to react with SO2 and HCl that are formed during the reaction. After the addition was complete, the solution was stirred for 3 hours at room temperature and then heated to reflux. After 3.5 hours of reflux, it was cooled to room temperature. Solvent was distilled at atmospheric pressure because removal under reduced pressure caused severe bumping. After most of the solvent was removed, the residue was transferred to a 1000 ml flask equipped with a distillation head. The product was then vacuum distilled.

1. customTo a 2000 ml four-necked reaction flask, equipped with a magnetic stirrer
2. additionthermometer, addition funnel, condenser
3. additionabove was added over approximately 20 minutes
4. customThe reaction temperature was kept below 20° C. with an ice/water bath
5. customThe nitrogen sweep was connected to a trap
6. customare formed during the reaction
7. additionAfter the addition
8. temperatureheated to reflux
9. temperatureAfter 3.5 hours of reflux
10. temperatureit was cooled to room temperature
11. distillationSolvent was distilled at atmospheric pressure because removal under reduced pressure
12. customAfter most of the solvent was removed
13. customthe residue was transferred to a 1000 ml flask
14. customequipped with a distillation head
15. distillationvacuum distilled