反应详情

温度

120 °C

A solution of 22.7 g of ethyl 4,4,4-trifluoro-3-amino-2-butenoate is added dropwise with stirring and cooling at 0-5° C. under a nitrogen atmosphere to 5.1 g of a previously introduced sodium hydride dispersion (60%) in 60 ml of n-methylpyrrolidine, and stirring is continued at 22° C. until the evolution of hydrogen has ceased. Then, 23.7 g of 2-ethoxycarbonylamino-3-fluoro-5-chloropyridine (Example H1) are added and the reaction mixture is heated for approx. 5 hours at 120° C. It is then cooled, 16.7 9 of methyl iodide are added dropwise, and stirring is continued overnight at 22° C. After the reaction mixture has been taken up in ethyl acetate, it is washed with ice-water, dried over sodium sulfate, filtered and evaporated. The residue obtained is recrystallized from ethyl acetate/n-hexane. This gives the desired title compound of m.p. 133-134° C.

1. stirringstirring
2. temperatureIt is then cooled
3. stirringstirring
4. washit is washed with ice-water
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customevaporated
8. customThe residue obtained
9. customis recrystallized from ethyl acetate/n-hexane