反应详情

197 g (1 mole) of 1-bromo-3,3-dimethyl-4-fluoro-2-butanone were slowly added dropwise to a boiling solution of 77 g (1.1 mols) of 1,2,4-triazole and 210 g (1.5 moles) of potassium carbonate in 500 ml of acetone such that, after removing the heating bath, the exothermic reaction kept the solution simmering. The mixture was then kept under reflux for a further 3 hours, the inorganic salts were filtered off and the filtrate was concentrated in vacuo. The residue was taken up in chloroform/water and the organic phase was separated off and evaporated. The residue which remained was distilled in vacuo and the distillate was crystallized with cyclohexane. 112 g (55% of theory) of 3,3-dimethyl-4-fluoro-1-(1,2,4-triazol-1-yl)-butan-2-one of melting point 59° C. were obtained. ##STR15##

1. customafter removing the heating bath
2. customthe exothermic reaction
3. temperatureunder reflux for a further 3 hours
4. filtrationthe inorganic salts were filtered off
5. concentrationthe filtrate was concentrated in vacuo
6. customthe organic phase was separated off
7. customevaporated
8. distillationThe residue which remained was distilled in vacuo
9. customthe distillate was crystallized with cyclohexane