反应详情

2.67 g (6 mmol) of 1-cyano-1-[N-methyl-N-(3-trifluoromethylphenyl)carbamoyl]-2-[imino(4,4-dimethyl-2-oxo-1-imidazolidinyl)methylamino]ethene hydrochloride are heated at 187°-189° C. under vacuum (4-6 mbar) for 10 min in a bath preheated to 190° C. After cooling, the solidified melt was mixed with 5 ml of 2N sodium hydroxide solution. 12 ml of diethyl ether/diisopropyl ether 5:1 were added. Stirring resulted in initial formation of two clear phases, from which crystals separated out. The mixture was stirred while cooling in ice for 1 hour, and the crystals were filtered off with suction, washed with water and taken up in 50 ml of CH2Cl2. The solution which formed was extracted successively three times with 5 ml of 0.5N NaOH each time and twice with 5 ml of water each time, dried over Na2SO4, filtered and evaporated. The residue was triturated with diisopropyl ether, filtered off with suction and dried as in Example 13. 0.82 g (=32.6% yield) of the compound I was obtained, melting point 209°-210° C.

1. custompreheated to 190° C
2. temperatureAfter cooling
3. customresulted in initial formation of two clear phases
4. customfrom which crystals separated out
5. stirringThe mixture was stirred
6. temperaturewhile cooling in ice for 1 hour
7. filtrationthe crystals were filtered off with suction
8. washwashed with water
9. customThe solution which formed
10. extractionwas extracted successively three times with 5 ml of 0.5N NaOH each time
11. dry with materialtwice with 5 ml of water each time, dried over Na2SO4
12. filtrationfiltered
13. customevaporated
14. customThe residue was triturated with diisopropyl ether
15. filtrationfiltered off with suction
16. customdried as in Example 13