反应详情

A solution of diethyl 2-{[(thien-3-yl)amino]methylene}malonate (43.4 g, 0.16 mol) in diphenyl ether (200 mL) in a 500 mL round bottom (RB) flask was degassed by three cycles of evacuation and nitrogen purge. The solution was then heated rapidly with a heating mantle to reflux and stirred at that temperature for 50 minutes. The heating mantle was removed and the yellow to brown solution was then stirred for 3 hours and was allowed to stand at room temperature for 16 hours, during which time a copious ppt appeared. The mixture was diluted with diethyl ether (300 mL) before collecting the solid by vacuum filtration. The collected solid was washed thoroughly with ether and dried in vacuo, leaving a white solid (21 g). More solid precipitated after the filtrate standing at room temperature overnight (7 g).

1. custompurge
2. temperatureThe solution was then heated rapidly with a heating mantle
3. temperatureto reflux
4. customThe heating mantle was removed
5. stirringthe yellow to brown solution was then stirred for 3 hours
6. waitto stand at room temperature for 16 hours, during which time
7. additionThe mixture was diluted with diethyl ether (300 mL)
8. custombefore collecting the solid
9. filtrationby vacuum filtration
10. washThe collected solid was washed thoroughly with ether
11. customdried in vacuo