反应详情

Under conditions of inert atmosphere, saturated with nitrogen, suspend 10.0 g of Z, N-[2-[[[5-(dimethylamino)methyl-2-furanyl]methyl]thio]ethyl]-N′-methyl-2-nitro-1,1-ethenediamine in 100 ml of anhydrous ethyl acetate (moisture<0.01%). Add dropwise to the mixture 21.95 g of hydrochloric acid in isopropanol (concentration 5.29% mol/mol) during 45 minutes, keeping the temperature at 25° C. Stirring vigorously, again in inert nitrogen atmosphere, a white precipitate is obtained. By operating again in a nitrogen-saturated atmosphere, wash and filter the precipitate with a mixture of ethyl acetate/isopropanol in 80:20 ratio and later with ethyl acetate alone. Dry the resulting precipitate in an oven at 40°-50° C. to remove the residual solvents and afterwards place it in a drier in-vacuo on phosphorus pentoxide, until a constant weight is obtained.

1. customat 25° C
2. customa white precipitate is obtained
3. washwash
4. filtrationfilter the precipitate
5. additionwith a mixture of ethyl acetate/isopropanol in 80:20 ratio
6. customDry the resulting precipitate in an oven at 40°-50° C.
7. customto remove the residual solvents
8. customuntil a constant weight is obtained