Oxalic Acid → 6-Chloro-5,7-difluoro-1,4-dihydroquinoxaline-2,3-dione
반응식
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([NH2:9])=[C:4]([NH2:10])[C:3]=1[F:11].[C:12](O)(=[O:16])[C:13](O)=[O:14]>Cl>[Cl:1][C:2]1[C:3]([F:11])=[C:4]2[C:5](=[CH:6][C:7]=1[F:8])[NH:9][C:13](=[O:14])[C:12](=[O:16])[NH:10]2참가 물질
4
실험 절차
A mixture of 230 mg (1.29 mmol) of 4-chloro-3,5-difluoro-1,2-phenylenediamine and 125 mg (1.38 mmol) of oxalic acid in 4 mL of 2N HCl was refluxed for 3 h and cooled to room temperature. The mixture was filtered and washed by water, dried to leave a brown solid (245 mg, 82%), mp>250° C. 1H NMR (DMSO-d6), 6.921 (d, 1, J=9.61), 12.143 (s, 1), 12.168 (s, 1). MS, 232 (M+, 100), 204 (80), 176 (40), 149 (70), 171 (80). HRMS calcd for C8H335ClF2N2O2, 231.9848, found 231.9851.
후처리
- temperaturewas refluxed for 3 h
- filtrationThe mixture was filtered
- washwashed by water
- customdried
출처 및 근거
- ORD 기록
- ord-f1011d0dbbc044e58501829eee3cb3e4
- 출처 데이터셋
- uspto-grants-1996_05
- 특허 번호
- US05514680
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