反应详情

Under inert atmosphere, 5 g of sodium salt of the β-oxo-3-pyridinepropanal, with HPLC purity of 99% (A %) and salt content of 25% (residue by calcination), and 8 mL hydrochloric acid in isopropanol in 50 mL toluene is suspended. 3.7 g (2-methyl-5-nitrophenyl)guanidine is added, and the mixture is stirred at room temperature for an hour. The mixture is refluxed for 18 hours, removing the water with a Dean Stark apparatus. Once completed the conversion, the suspension is cooled to 10° C., and the precipitate is filtrated; this is crushed in warm water, yielding, upon filtration and drying, 2.5 g of product with HPLC purity of 96% (A %), identified through GC-MS.

1. temperatureThe mixture is refluxed for 18 hours
2. customremoving the water with a Dean Stark apparatus
3. temperaturethe suspension is cooled to 10° C.
4. filtrationthe precipitate is filtrated
5. customthis is crushed in warm water
6. customyielding, upon filtration
7. customdrying