反应详情

10.9 g (0.1 mole) of propionamidine hydrochloride were suspended in 125 ml of water and 200 ml of benzene. 15.6 g (0.1 mole) of N-methyl-bis-(chlorocarbonyl)-amine in 100 ml of dry benzene and 18 g (0.45 mole) of sodium hydroxide dissolved in 100 ml of water were simultaneously slowly added dropwise from two dropping funnels, with vigorous stirring. The reaction took place exothermically. The mixture was stirred for a further hour, the aqueous phase was separated off and acidified with glacial acetic acid and the mixture was evaporated in vacuo. The residue was repeatedly extracted by boiling with ethyl acetate. The solution was concentrated in vacuo and cooled. The precipitate was filtered off. 7.8 g (50%) of 1-methyl-4-ethyl-tetrahydro-1,3,5-triazine-2,6-dione were obtained as colorless needles of melting point 202°-203° C.

1. additionwere simultaneously slowly added dropwise from two dropping funnels, with vigorous stirring
2. customthe aqueous phase was separated off
3. customthe mixture was evaporated in vacuo
4. extractionThe residue was repeatedly extracted
5. concentrationThe solution was concentrated in vacuo
6. temperaturecooled
7. filtrationThe precipitate was filtered off