Reaktion #937104

Reaktionsgleichung

nitric acid

sulfuric acid

3-(2,4-difluorophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine

compound 1-10

3-(2,4-difluorophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine

→

3-(2,4-difluoro-5-nitrophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine

Ausbeute 96.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter completion of the reaction
2. 2
   Extraktionfollowed by extraction with ethyl acetate
3. 3
   WaschenThe organic layer was washed with water
4. 4
   Trocknensaturated sodium chloride solution, dried with anhydrous magnesium sulfate
5. 5
   Einengenconcentrated

Vorschrift

To 85 ml of concentrated sulfuric acid was added 7.0 g of 3-(2,4-difluorophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-10) at 5° C. Furthermore, 9 ml of 70% nitric acid was added, and the mixture was stirred at 5° to 10° C. for 8 hours. After completion of the reaction, the reaction mixture was added to ice water, followed by extraction with ethyl acetate. The organic layer was washed with water and then saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography, which afforded 7.76 g (yield, 96%) of 3-(2,4-difluoro-5-nitrophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-16; m.p., 93.2° C.).

Quelle