反应详情

温度

250 °C

Diethyl 2-({[2-(trifluoromethyl)phenyl]amino}methylene)malonate (compound of formula (IV)), 69.73 g, 210.5 mmol) was taken into Dowtherm A (350 mL) and brought to reflux (˜250° C.) with the removal of ethanol that was formed during the reaction for 45 min. The reaction was allowed to cool to approximately 100° C. then carefully poured into hexane (1 L) and allowed to cool overnight. A white solid precipitated which was filtered and dried to afford the title compound as a white solid (55.04 g, 91.7%). MS ESI (m/z) 286 ([M+H]+); MS ESI (m/z) 284 ([M−H]−).

1. customwith the removal of ethanol that
2. customwas formed during the reaction for 45 min
3. temperatureto cool to approximately 100° C.
4. temperatureto cool overnight
5. customA white solid precipitated which
6. filtrationwas filtered
7. customdried