Nitric Acid → HCID 19365540、化合物

反応式

S(=O)(=O)(O)O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:14](=[O:24])[N:15]([CH3:23])[C:16]([C:19]([F:22])([F:21])[F:20])=[CH:17][N:18]=2)=[C:9]([F:25])[CH:8]=1.[N+:26]([O-])([OH:28])=[O:27]>>[Cl:6][C:7]1[C:12]([N+:26]([O-:28])=[O:27])=[CH:11][C:10]([C:13]2[C:14](=[O:24])[N:15]([CH3:23])[C:16]([C:19]([F:22])([F:20])[F:21])=[CH:17][N:18]=2)=[C:9]([F:25])[CH:8]=1

参加物

反応物 3

HCID 944Nitric Acid

HCID 1118Sulfuric Acid

HCID 19365486HCID 19365486、化合物2 回

生成物 1

HCID 19365540HCID 19365540、化合物収率 95%

実験手順

To 3.3 ml of concentrated sulfuric acid was added 0.50 g of 3-(4chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-11) at 5° C. Furthermore, 0.17 ml of 61% nitric acid was added, and the mixture was stirred at room temperature for 1 hour. 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 0.55 g (yield, 95%) of 3-(4-chloro-2-fluoro-5-nitrophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-17; m.p., 98.3° C.).