反应详情

A mixture of 16.2 parts of 3-(2-chloroethyl)-6-nitro-2,4(1H,3H)-quinazolinedione, 15 parts of 4-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]piperidine, 10 parts of sodium hydrogen carbonate, 0.1 parts of potassium iodide and 135 parts of N,N-dimethylformamide was stirred and heated overnight at 100°-120° C. The reaction mixture was cooled and poured onto water. Stirring was continued till complete precipitation. The precipitate was filtered off and dissolved in trichloromethane. The thus formed emulsion was dried, filtered and evaporated. The residue was crystallized from acetonitrile, yielding 18.6 parts (64%) of 3-[2-[4-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-1-piperidinyl]ethyl]-6-nitro-2,4(1H,3H)-quinazolinedione; mp. 250.9° C. (28).

1. temperatureheated overnight at 100°-120° C
2. temperatureThe reaction mixture was cooled
3. additionpoured onto water
4. stirringStirring
5. customwas continued till complete precipitation
6. filtrationThe precipitate was filtered off
7. dissolutiondissolved in trichloromethane
8. customThe thus formed emulsion was dried
9. filtrationfiltered
10. customevaporated
11. customThe residue was crystallized from acetonitrile