反应详情

温度

130 °C

3-(3,5-Dimethyl-4-isoxazolyl)aniline (for a preparation see Intermediate 2, 80 g, 420 mmol) and diethyl ethoxymethylenemalonate (92 g, 425 mmol) were mixed together and heated to 130° C. for 20 minutes, liberating ethanol, which was evaporated under reduced pressure. The reaction mixture was poured into iPr2O (1 L) and the resulted precipitate filtered off and washed with iPr2O. The resulting solid was recrystallised from acetonitrile to give the title compound as a brown solid (78 g, 52%).

1. additionwere mixed together
2. customliberating ethanol, which was evaporated under reduced pressure
3. additionThe reaction mixture was poured into iPr2O (1 L)
4. filtrationthe resulted precipitate filtered off
5. washwashed with iPr2O
6. customThe resulting solid was recrystallised from acetonitrile