反应详情

3.1 ml of a 6.6 molar solution of HCl in ether were added dropwise to a suspension of 8.17 g (20 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 48 ml of ethanol at room temperature, and the mixture was stirred at 1°-3° C. for 1 hour. The solid was then filtered off with suction, washed with ether and dried at room temperature in vacuo (4-6 mbar) for 20 hours. 8.34 g (=90.7% yield) of pure 1-cyano-1-[N-methyl-N-(3-trifluoromethylphenyl)carbamoyl]-2-[imino-(4,4-dimethyl-2-oxo-1-imidazolidinyl)methylamino]ethene hydrochloride were obtained, melting point 180°-181° C. (=transition point; substance resolidifies); C18H20ClF3N6O2 (444.86)

1. filtrationThe solid was then filtered off with suction
2. washwashed with ether
3. customdried at room temperature in vacuo (4-6 mbar) for 20 hours