反应详情

Under inert atmosphere, 16 g sodium salt of β-oxo-3-pyridinepropanal, with HPLC purity of 99% (A %) and 25% salt content (residue by calcination), and 11.7 g (2-methyl-5-aminophenyl)guanidine in 115 mL n-butanol is suspended. 9 mL acetic acid is added, and the mixture is stirred at room temperature for an hour. 6 g potassium hydroxide is added portionwise, and the mixture is refluxed for 18 hours, removing the water with a Dean Stark apparatus. Once completed the conversion, the suspension is cooled and the organic layer is washed with water. The organic layer is concentrated to a small volume, and toluene is added. The precipitate is filtrated, yielding, upon drying, 15.5 g of product with HPLC purity of 99.2% (A %), identified through LC-MS and

1. temperaturethe mixture is refluxed for 18 hours
2. customremoving the water with a Dean Stark apparatus
3. temperaturethe suspension is cooled
4. washthe organic layer is washed with water
5. concentrationThe organic layer is concentrated to a small volume, and toluene
6. additionis added
7. filtrationThe precipitate is filtrated
8. customyielding
9. customupon drying