反应详情

温度

130 °C

In a heavy walled round bottom flask with screw top were combined ethyl 5-butoxy-1,3-oxazole-2-carboxylate (2.53 g, 11.88 mmol) and 1-(4-fluorobenzyl)-5,6-dihydropyridin-2-(1H)-one (1.22 g, 5.94 mmol; see Example 1, Step 3) and trifluoroacetic acid (0.46 mL, 5.94 mmol). The vessel was sealed and placed in an oil bath heated to 130° C. The reaction mixture was stirred for 3 days. The dark brown reaction mixture was cooled and a crystalline precipitate formed. The mixture was diluted with ether and the solids collected by filtration and washed with ether to give the product as tan shiny plates. Further product can be obtained by evaporating the mother liquor, adding more trifluoroacetic acid and re-heating the mixture.

1. customIn a heavy walled round bottom flask with screw top were combined
2. customThe vessel was sealed
3. customplaced in an oil bath
4. temperatureThe dark brown reaction mixture was cooled
5. customa crystalline precipitate formed
6. filtrationthe solids collected by filtration
7. washwashed with ether
8. customto give the product as tan shiny plates
9. customFurther product can be obtained
10. customby evaporating the mother liquor
11. additionadding more trifluoroacetic acid
12. temperaturere-heating the mixture