Hydrochloric Acid → 4-Chloro-2-methyl-3-(trifluoromethyl)aniline
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8]C(=O)C(C)(C)C)=[C:4]([CH3:15])[C:3]=1[C:16]([F:19])([F:18])[F:17].Cl>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([CH3:15])[C:3]=1[C:16]([F:17])([F:18])[F:19]参加物
4
実験手順
N-(4-Chloro-2-methyl-3-trifluoromethylphenyl)-2,2-dimethyl-propionamide 1.0 g, 3.4 mmol) was added to a 1:1 mixture (15 mL) of concentrated HCl and ethanol and heated at reflux for overnight. The reaction was cooled and concentrated in vacuo to give a tan solid which was then partitioned between EtOAc and saturated NaHCO3. The organic layer was separated, washed with water, brine, dried (Na2SO4), filtered and concentrated to give compound 760C (0.54 g, 76%) as a brown oily solid.
後処理
- temperatureheated
- temperatureat reflux for overnight
- temperatureThe reaction was cooled
- concentrationconcentrated in vacuo
- customto give a tan solid which
- customwas then partitioned between EtOAc and saturated NaHCO3
- customThe organic layer was separated
- washwashed with water, brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-4216203445d844fe9722df4d03ab00ce
- 出典データセット
- uspto-grants-2008_12
- 特許番号
- US07470797B2
反応ノート
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