反应详情

111.75 g (75 ml, 0.98 mol) of trifluoroacetic acid are added to 100 g (0.613 mol) of sodium salt of ethyl cyanopyruvate (prepared in analogy to Borsche and Manteuffel, Liebigs Ann. 1934, 512, 97) in 2.5 l of dioxane under argon with efficient stirring at room temperature, and the mixture is stirred for 10 minutes during which much of the precursor dissolves. Then 85.93 g (0.613 mol) of 2-fluorobenzylhydrazine are added, and the mixture is heated under reflux overnight. After cooling, the crystals of sodium trifluoroacetate which have separated out are filtered off with suction and washed with dioxane, and the solution is reacted further as it is.

1. stirringthe mixture is stirred for 10 minutes during which much of the precursor
2. dissolutiondissolves
3. temperaturethe mixture is heated
4. temperatureunder reflux overnight
5. temperatureAfter cooling
6. customthe crystals of sodium trifluoroacetate which have separated out
7. filtrationare filtered off with suction
8. washwashed with dioxane
9. customthe solution is reacted further as it