反应详情

A 250 ml round-bottomed flask, Teflon stirrer, reflux condenser, and gas inlet were oven-dried for 12 hours at 160° C. The apparatus was rapidly assembled, flushed with dry nitrogen gas, and allowed to cool to room temperature. After cooling, the flask was charged with malonic acid (110 mmole), pyridine (75 ml), 2,3-dichlorobenzaldehyde (17.50 g, 100 mmole) and piperidine (2 ml, 20 mmole). The reaction mixture was stirred and brought to relux. After 16 hours of stirring under reflux, the reaction mixture was cooled to room temperature and poured onto a mixture of ice (100 ml) and concentrated hydrochloric acid (100 ml) resulting in the precipitation of a white solid to form a slurry. The resulting slurry was stirred for 2 hours, filtered, washed with cold water (2×250 ml), and dried in vacuo to give 20.01 g (92%) of 2,3-dichlorocinnamic acid.

1. temperatureA 250 ml round-bottomed flask, Teflon stirrer, reflux condenser, and gas inlet
2. customwere oven-dried for 12 hours at 160° C
3. customflushed with dry nitrogen gas
4. temperatureAfter cooling
5. stirringAfter 16 hours of stirring
6. temperatureunder reflux
7. temperaturethe reaction mixture was cooled to room temperature
8. customresulting in the precipitation of a white solid
9. customto form a slurry
10. stirringThe resulting slurry was stirred for 2 hours
11. filtrationfiltered
12. washwashed with cold water (2×250 ml)
13. customdried in vacuo