Nitric Acid → Ethyl 3,5-difluoro-2-nitrobenzoate
反応式
[N+:1]([O-:4])(O)=[O:2].OS(O)(=O)=O.[CH2:10]([O:12][C:13](=[O:22])[C:14]1[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([F:21])[CH:15]=1)[CH3:11]>>[CH2:10]([O:12][C:13](=[O:22])[C:14]1[CH:19]=[C:18]([F:20])[CH:17]=[C:16]([F:21])[C:15]=1[N+:1]([O-:4])=[O:2])[CH3:11]参加物
4
実験手順
10.0 mL of conc. HNO3 at 0° C. was slowly treated with 20.0 mL of conc. H2SO4, then 7.6 g (40 mmol) of 3,5-difluoro-benzoic acid ethyl ester. The reaction mixture was warmed up to room temperature and stirred overnight. This mixture was poured into a beaker containing ice. The resulting mixture was extracted with ethyl acetate, washed with cold water and evaporated to produce 7.4 g (32 mmol, 80%) of 3,5-difluoro-2-nitro-benzoic acid ethyl ester. LCMS: 232 (M+1)+.
後処理
- additionThis mixture was poured into a beaker
- additioncontaining ice
- extractionThe resulting mixture was extracted with ethyl acetate
- washwashed with cold water
- customevaporated
出典と根拠
- ORDレコード
- ord-99aaaadd6cd74df9b409fb7699892808
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07893267B2
反応ノート
読み込み中…