反应详情

温度

60 °C

A mixture of 7.04 g of methyl 3-(8-trifluoromethyl-4-quinolylamino)-2-thiophene-carboxylate, 5.5 g of 4-(4-chlorophenyl)-1-piperazine ethanol and 50 ml of anhydrous toluene was refluxed for an hour while passing condensed toluene through a column filled with siliporite and after cooling the mixture to 60° C, 150 ml of sodium hydride were added. The mixture was refluxed with stirring for 16 hours and the toluene was distilled. The residue was extracted with methylene chloride, was washed and dried. The product was crystallized from 95% ethanol, iced and vacuum filtered. The precipitate was washed with ethanol and dried to obtain 8.6 g of 2-[4-(4-chlorophenyl)-1-piperazinyl]-ethyl 3-(8-trifluoromethyl 4-quinolylamino)-2-thiophene-carboxylate melting at 155° C.

1. temperaturewas refluxed for an hour
2. additionfilled with siliporite and
3. temperatureThe mixture was refluxed
4. distillationthe toluene was distilled
5. extractionThe residue was extracted with methylene chloride
6. washwas washed
7. customdried
8. customThe product was crystallized from 95% ethanol
9. filtrationiced and vacuum filtered
10. washThe precipitate was washed with ethanol
11. customdried