반응 #82072

반응 방정식

ethanol

3,4,5-trifluoro-1,2-phenylenediamine

oxalic acid

→

pure title compound

수율 36.0%

5,6,7-Trifluoro-1,4-dihydro-2,3-quinoxalinedione

수율 36.0%

용매

HCl

반응 조건

후처리

1. 1
   온도to reflux
2. 2
   여과The mixture is filtered
3. 3
   기타to yield 139 mg (37%) of crude title compound
4. 4
   기타An analytical sample is prepared
5. 5
   온도Upon cooling
6. 6
   기타brown rod-like crystals were formed which
7. 7
   여과are filtered
8. 8
   기타dried in vacuo

실험 절차

To a brown solution of 3,4,5-trifluoro-1,2-phenylenediamine (285 mg, 1.75 mmol) in aqueous 2N HCl (10 mL) is added oxalic acid (221 mg, 1.75 mmol). The brown mixture is brought to reflux and stirred under N2 overnight. The mixture is filtered to yield 139 mg (37%) of crude title compound. An analytical sample is prepared by dissolving 42 mg of this brown powder in 2.5 mL boiling ethanol. Upon cooling, brown rod-like crystals were formed which are filtered and dried in vacuo to yield 15 mg (36%) of pure title compound: 1H NMR (DMSO-d6), 6.91 (m, 1H), 12.02 (s, 1H), 12.19 (s, 1H); analysis calculated for C8H3F3N2O2 : C, 44.46; H, 1.40; N, 12.96. Found: C, 44.42; H, 1.16; N, 12.76.

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