反应详情

In an analogous manner to the description in Example 22, 1.35 ml of a 6.6 molar solution of HCl in ether were added to a solution of 8 mmol of the compound I in 25 ml of ethyl acetate and 5 ml of methanol, and the mixture was then evaporated in vacuo. The viscous oily residue was dissolved in 20 ml of boiling acetone, whereupon a crystalline precipitate separated out after a few minutes. After stirring while cooling in an icebath for 30 min, the solid was filtered off with suction, washed with acetone and ether and dried as described in Example 13. 3.28 g (92.3% yield) of pure 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)pyrimidine-5-carboxylic acid N-methyl-N-(3-trifluoromethylphenyl)amide hydrochloride were obtained, melting point 210°-211° C.

1. customthe mixture was then evaporated in vacuo
2. dissolutionThe viscous oily residue was dissolved in 20 ml of boiling acetone, whereupon a crystalline precipitate
3. customseparated out after a few minutes
4. temperaturewhile cooling in an icebath for 30 min
5. filtrationthe solid was filtered off with suction
6. washwashed with acetone and ether
7. customdried