反应详情

A solution of 1.634 g (4 mmol) of 1-cyano-1-[N-methyl-N-(3-trifluoromethylphenyl)carbamoyl]-2-[imino(4,4-dimethyl-2-oxo-1-imidazolidinyl)methylamino]ethene (compound IV) in 3 ml of formic acid (98-100% strength) was heated at 50° C. for 2 hours. The formic acid was then stripped off in vacuo, the residue was taken up in dichloromethane, 20 ml of water were added, and the pH was adjusted to between 9 and 10 with dilute sodium hydroxide solution. The organic phase was separated off. The aqueous phase was extracted twice more with dichloromethane. The combined dichloromethane extracts were washed successively with 2 ml of 0.5N NaOH and twice with water, dried with MgSO4 and evaporated in vacuo. The remaining solid residue was mixed with ether/heptane 1:1 and filtered off with suction. After drying (compare Example 13), 0.93 g (=56.9% yield) of pure 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)pyrimidine-5-carboxylic acid N-methyl-N-(3-trifluoromethylphenyl) amide was obtained, melting point 210°-211° C.; TLC in CH2Cl2 /C2 H5OH=10:1.

1. customThe organic phase was separated off
2. extractionThe aqueous phase was extracted twice more with dichloromethane
3. washThe combined dichloromethane extracts were washed successively with 2 ml of 0.5N NaOH and twice with water
4. dry with materialdried with MgSO4
5. customevaporated in vacuo
6. additionThe remaining solid residue was mixed with ether/heptane 1:1
7. filtrationfiltered off with suction
8. customAfter drying (compare Example 13)