反应详情

To a suspension of 10.5 g of sodium salt of cyanoacetone in 200 ml of dimethylformamide 9.0 ml of carbon disulphide are gradually added while stirring cooling in ice and keeping under nitrogen, succeeded by 4.5 g of sodium hydride dispersion. After stirring for an hour with cooling, 8.4 ml of chloroacetone are added dropwise under the same reaction conditions. After stirring for another hour, 0.4 g of powdered NaOH are added and finally, after again stirring for another 0.5 hour, 8.0 ml of ethyl iodide under the same conditions. After stirring, the reaction mixture for again another hour and leaving to stand overnight it is poured 1 l of ice water and extracted with diethyl ether. The organic phase is washed with water three times, dried, treated with charcoal, filtered and evaporated. After recrystallisation from isopropanol, the residue yields the desired product in a yield of 9.54 g; melting-point 51°-52° C.

1. additionare gradually added
2. temperaturecooling in ice
3. stirringAfter stirring for an hour
4. temperaturewith cooling
5. stirringAfter stirring for another hour
6. stirringfinally, after again stirring for another 0.5 hour
7. stirringAfter stirring
8. waitthe reaction mixture for again another hour
9. customleaving
10. extractionextracted with diethyl ether
11. washThe organic phase is washed with water three times
12. customdried
13. additiontreated with charcoal
14. filtrationfiltered
15. customevaporated
16. customAfter recrystallisation from isopropanol