Water → 5-Fluoro-3-methyl-2-nitrobenzoic acid
反応式
[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]参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-40611bb438ed41998c17be98b3199c19
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08071623B2
反応ノート
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