反应详情

温度

240 °C

Diphenyl ether (870 mL) was heated to 240° C. then diethyl 2-[[(4-bromophenyl)amino]methylidene]propanedioate (75 g, 219.18 mmol) added portionwise. The mixture was stirred at 240° C. for 60 minutes in a flask fitted with clean-stark apparatus. After cooling (25° C.) a crystallized solid was formed. The mixture was diluted with Et2O and the solid was collected by filtration, washed with Et2O and dried to afford the desired material (59.9 g) as a beige crystallized solid, which was used without purification or characterisation.

1. customfitted with clean-stark apparatus
2. temperatureAfter cooling (25° C.) a crystallized solid
3. customwas formed
4. filtrationthe solid was collected by filtration
5. washwashed with Et2O
6. customdried