反应详情

To the solution of 4 g of malonitrile in 50 mL of dimethylformamide in several portions 2.4 g of sodium hydride 60% oily dispersion is added. To the clear solution 8 g of 5-dimethylamino-isatoic anhydride is added and the mixture is stirred at room temperature for 10 hours. The mixture is diluted with 70 mL of water and extracted with 2×30 mL of ethyl acetate. The aqueous phase is evaporated in vacuum, the solid residue is dissolved in 20 mL of water, the pH is adjusted to 6 with acetic acid. The precipitated material is filtered off, and washed with water. After drying 6.5 g of the title compound is obtained, m.p.: 360° C.

1. extractionextracted with 2×30 mL of ethyl acetate
2. customThe aqueous phase is evaporated in vacuum
3. dissolutionthe solid residue is dissolved in 20 mL of water
4. filtrationThe precipitated material is filtered off
5. washwashed with water
6. dry with materialAfter drying 6.5 g of the title compound
7. customis obtained