反应详情

温度

70 °C

A mixture of 2.45 g (6 mmol) of compound IV, 820 mg (5 mmol) of trichloroacetic acid and 4.25 ml of glacial acetic acid was stirred at 70° C. for 2 hours and subsequently evaporated in vacuo. The remaining residue was taken up in 100 ml of ethyl acetate and extracted successively twice each with 20 ml of 2N NaOH each time and 10 ml of water each time. The solution was dried over MgSO4 and then filtered and evaporated in vacuo. The residue was dissolved in 25 ml of ether, whereupon crystals separated out. The mixture was stirred at room temperature for 30 minutes and then evaporated in vacuo. The crystalline residue was suspended in diisopropyl ether, filtered off with suction and dried in vacuo at 100° C. for 15 hours. 1.36 g (=55.5% yield) of pure 4-amino-2-(4,4-dimethyl-2-oxo-1-imidazolidinyl)-pyrimidine-5-carboxylic acid N-methyl-N-(3-trifluoromethylphenyl)amide were obtained, melting point 209°-210° C.

1. customsubsequently evaporated in vacuo
2. extractionextracted successively twice each with 20 ml of 2N NaOH each time and 10 ml of water each time
3. dry with materialThe solution was dried over MgSO4
4. filtrationfiltered
5. customevaporated in vacuo
6. dissolutionThe residue was dissolved in 25 ml of ether, whereupon crystals
7. customseparated out
8. stirringThe mixture was stirred at room temperature for 30 minutes
9. customevaporated in vacuo
10. filtrationfiltered off with suction
11. customdried in vacuo at 100° C. for 15 hours