反应详情

A solution of 285.5 mg (1.5 mmol) of p-toluenesulfonic acid hydrate in 10 ml of acetonitrile was added to a suspension of 613 mg (1.5 mmol) of compound I in 4 ml of acetonitrile at room temperature. The resulting solution (pH 3-4) was stirred at room temperature for 20 min and evaporated in vacuo. Ether was added to the residue. This resulted in crystallization of a substance which, after stirring at room temperature for 20 min, was filtered off with suction and washed with ether. Drying (5-6 mbar, 80° C., 8 hours) resulted in 820 mg (=94.1% yield) of pure 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)pyrimidine-5-carboxylic acid N-methyl-N-(3-trifluoromethylphenyl)amide p-toluenesulfonate, melting point 168°-170° C.

1. customevaporated in vacuo
2. additionEther was added to the residue
3. customThis resulted in crystallization of a substance which
4. filtrationwas filtered off with suction
5. washwashed with ether
6. customDrying (5-6 mbar, 80° C., 8 hours)