Methanol → Methyl 3-nitro-5-(trifluoromethyl)benzoate
反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:12]=1)[C:7]([OH:9])=[O:8])([O-:3])=[O:2].[CH3:17]O>>[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([C:13]([F:14])([F:15])[F:16])[CH:12]=1)[C:7]([O:9][CH3:17])=[O:8])([O-:3])=[O:2]参加物
3
実験手順
3-Nitro-5-(trifluoromethyl)benzoic acid (25.0 g, 106.3 mmol) was dissolved in methanol (60 mL) which was bubbled with hydrochloric acid gas for 1 h. The reaction was allowed to stir at room temperature overnight and concentrated. The crude product was dissolved in ethyl acetate, washed with water (2×), brine (2×) dried over sodium sulfate and concentrated. Flash chromatography on silica gel afforded 23.4 g (88%) of the desired compound. 1H-NMR (CDCl3, 500 MHz) δ 9.02 (s, H), 8.66 (s, 1H), 8.61 (s, 1H), 4.03 (s, 3H).
後処理
- customwas bubbled with hydrochloric acid gas for 1 h
- concentrationconcentrated
- dissolutionThe crude product was dissolved in ethyl acetate
- washwashed with water (2×), brine (2×)
- dry with materialdried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-0cf66fe26f434207a5602f8cd5c2609b
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08383821B2
反応ノート
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