反应详情

2-(Trimethylsilyl)ethyl 2-ethoxymethylenecyanoacetate (10.0 g, 41.4 mmol) and benzaldehyde-phenylhydrazone (8.13 g, 41.4 mmol) were combined in 50 mL xylenes under N2 and heated at reflux for 5 h, cooled to room temperature, then treated with hexane (50 mL) and allowed to stir overnight. The precipitate was filtered off, washed with hexane and dried to afford 5.46 g of crude product. Purification by chromatography afforded 2.69 g (16%) of 2-(trimethylsilyl)ethyl 3-(N′-benzylidene-N-phenylhydrazino)-2-cyanoacrylate, as a white solid.

1. temperatureheated
2. temperatureat reflux for 5 h
3. filtrationThe precipitate was filtered off
4. washwashed with hexane
5. customdried
6. customto afford 5.46 g of crude product
7. customPurification by chromatography