反应详情

温度

100 °C

2-Oxopropanal methylhydrazone (8.18 mmol, 819 mg) synthesized in Reference Synthetic Example 1 and (3,4-dimethylphenyl)(oxo)acetaldehyde (7.57 mmol, 1.227 g) synthesized in Reference Synthetic Example 5 were dissolved in acetic acid (30 mL) and stirred at 100° C. for about 5 hours. Then, the solvent was evaporated, and the residue was dried by means of a vacuum pump and subjected to silica gel column chromatography (n-hexane/AcOEt=2/1, and 4/1) to give the crude product. The crude product was stirred with CHCl3/n-hexane for a while, and then recovered by filtration. The filtered solid was combined with a solid obtained by silica gel thin layer chromatography purification (n-hexane/AcOEt=4/1) of the filtrate to give the desired product as an orange solid (237.5 mg, yield 13%).

1. customsynthesized in Reference Synthetic Example 5
2. customThen, the solvent was evaporated
3. customthe residue was dried by means of a vacuum pump
4. customto give the crude product
5. filtrationrecovered by filtration
6. customobtained by silica gel thin layer chromatography purification (n-hexane/AcOEt=4/1) of the filtrate