Water → 5-Fluoro-3-methyl-2-nitrobenzoic acid
반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([CH3:11])[CH:10]=1)[C:5]([OH:7])=[O:6].[N+:12]([O-])([O-:14])=[O:13].[K+].O>OS(O)(=O)=O>[F:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[C:4]([CH:3]=1)[C:5]([OH:7])=[O:6]참가 물질
5
실험 절차
To a solution of 3-fluoro-5-methylbenzoic acid (1.0 eq.) in conc. H2SO4 was added slowly KNO3 (1.1 eq.) at 0° C. The mixture was stirred at RT for 1 h and then slowly poured into iced water. After stirring to until the ice has completely melted, the white precipitation was filtered, washed with cold water and dried under reduced pressure. The white solid was used without further purification for the next step. 1H NMR (400 MHz, DMSO, 300K) δ 14.08 (1H, br. s), 7.65 (2H, m), 2.30 (3H, s).
후처리
- customthe white precipitation
- filtrationwas filtered
- washwashed with cold water
- customdried under reduced pressure
- customThe white solid was used without further purification for the next step
출처 및 근거
- ORD 기록
- ord-40611bb438ed41998c17be98b3199c19
- 출처 데이터셋
- uspto-grants-2011_12
- 특허 번호
- US08071623B2
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