反应详情

16.00 g (0.06 mol) of ethyl-6-[(dimethylamino)methylene]-1-methyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate were dissolved in 600 mL of ethanol and 3.90 g of sodium ethylate, and 5.44 g of guanidine hydrochloride were added consecutively. The solution was stirred at reflux for 12 hours. The solvent was then evaporated, the residue redissolved with dichloromethane and washed with water. The organic layer was then dried over anhydrous Na2SO4 and concentrated. The residue was triturated with diethyl ether and the product collected by filtration (85% yield as a white solid).

1. temperatureat reflux for 12 hours
2. customThe solvent was then evaporated
3. dissolutionthe residue redissolved with dichloromethane
4. washwashed with water
5. dry with materialThe organic layer was then dried over anhydrous Na2SO4
6. concentrationconcentrated
7. customThe residue was triturated with diethyl ether
8. filtrationthe product collected by filtration (85% yield as a white solid)