反应详情

A mixture of 5-amino-6-fluoro-3-methyl-1,2-benzisoxazole (4.85 g, 0.029 mol) and 2-dimethylamino-4-(trifluoromethyl)-6H-1,3-oxazin-6-one (6.70 g, 0.0320 mol) in acetic acid is refluxed for 90 minutes, cooled to room temperature, and poured into an ice-water mixture. The resultant aqueous mixture is filtered to obtain a solid. The solid is air-dried and dissolved in ethyl acetate. The resultant organic solution is washed with brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product as a yellow solid (7.00 g, mp 235-237° C.) which is identified by NMR spectral analyses.

1. temperatureis refluxed for 90 minutes
2. filtrationThe resultant aqueous mixture is filtered
3. customto obtain a solid
4. customThe solid is air-dried
5. dissolutiondissolved in ethyl acetate
6. washThe resultant organic solution is washed with brine
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated in vacuo