反应详情

4N hydrochloric acid was added dropwise to a stirred suspension of 45.5 g (111.4 mmol) of 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)pyrimidine-5-carboxylic acid N-methyl-N-(3-trifluoromethylphenyl)amide (compound I) in 810 ml of 1,2-dimethoxyethane at room temperature until the pH was constant at 3.0. 28.4 ml of 4N hydrochloric acid were required for this. The resulting solution was stirred for 30 min (at room temperature) and then evaporated in vacuo. The remaining viscous oily residue was dissolved in 150 ml of boiling acetone, whereupon the formation of a crystalline precipitate immediately started. After cooling in an icebath for 30 min, the crystals were filtered off with suction, washed with acetone and ether and dried at 100° C. in vacuo (180 mbar) for 17 hours. 46.7 g (=94.2% 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. customevaporated in vacuo
2. dissolutionThe remaining viscous oily residue was dissolved in 150 ml of boiling acetone, whereupon the formation of a crystalline precipitate
3. temperatureAfter cooling in an icebath for 30 min
4. filtrationthe crystals were filtered off with suction
5. washwashed with acetone and ether
6. customdried at 100° C. in vacuo (180 mbar) for 17 hours