反应详情

To a stirred slurry of 12.45 g (0.11mole) of creatinine in 100 ml of dry DMF is added 16.41 g (0.1 mole) of m-nitrophenyl isocyanate (previously recrystallized from benzene-pentane). After nine hours, ice water is gradually added until crystallization occurres. A large excess of ice water precipitates the product as gummy crystals which then crystallize. The crude product is allowed to air dry for several days. Recrystallization from THF-H2O followed by THF gives pure product, 1-(1-methyl-4-oxo-2-imidazolidinylidene)-3-m-nitrophenyl urea; m.p. 182°-188° C. sl. dec.

1. custompreviously recrystallized from benzene-pentane)
2. additionice water is gradually added until crystallization
3. customA large excess of ice water precipitates the product as gummy crystals which
4. customthen crystallize
5. customto air dry for several days
6. customRecrystallization from THF-H2O