反应详情

温度

10 °C

A solution of NaNO2 (0.36 mole) in H2O (50 ml) was added to a solution of intermediate (3) (0.34 mole) in acetic acid (700 ml) and HCl (102 ml), stirred at 10° C. The reaction mixture was stirred for 80 minutes at 10° C. A powdered mixture of sodium acetate (1.02 mole) and diethyl(1,3-dioxo-1,3-propanediyl)biscarbamate (0.374 mole) was added and the reaction mixture was stirred for 40 minutes. The reaction mixture was poured out onto crushed ice. The precipitate was filtered off, washed with water, taken up into CH2Cl2, and the layers were separated. The organic layer was dried, filtered and the solvent evaporated, yielding 138.5 g (84%) of diethyl N,N′-[2-[[3,5-dichloro-4-(1-cyano-1-methylethyl)phenyl]hydrazono]-1,3-dioxo-1,3-propanediyl]dicarbamate (intermediate 4).

1. stirringThe reaction mixture was stirred for 80 minutes at 10° C
2. additionwas added
3. stirringthe reaction mixture was stirred for 40 minutes
4. additionThe reaction mixture was poured out
5. customonto crushed ice
6. filtrationThe precipitate was filtered off
7. washwashed with water
8. customthe layers were separated
9. customThe organic layer was dried
10. filtrationfiltered
11. customthe solvent evaporated