反应详情

1-chloro-1-cyclohexene (5.8 g; 0.049 mol) was added to lithium (1.1 g; 0.049 mol) in diethyl ether (50 ml) in a single portion. After stirring overnight at room temperature, stirring was continued for 7 more hours with reflux. After cooling, ethyl-3-(N,N-dimethylamino)propionate (3.0 g; 0.021 mol) was added and as a result of the exothermic reaction refluxing occurred. After cooling to room temperature and stirring for another 30 minutes 100 ml of water was added. The water layer was separated off and extracted with diethyl ether. The combined ether layer was dried (K2CO3), filtered and evaporated. The yield was 4.5 g (83%).

1. stirringstirring
2. temperaturewith reflux
3. temperatureAfter cooling
4. customas a result of the exothermic reaction
5. temperaturerefluxing
6. temperatureAfter cooling to room temperature
7. additionwas added
8. customThe water layer was separated off
9. extractionextracted with diethyl ether
10. dry with materialThe combined ether layer was dried (K2CO3)
11. filtrationfiltered
12. customevaporated