Hydrochloric Acid → 4-Chloro-2-methyl-3-(trifluoromethyl)aniline
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-047e7f6c68f845a08eb34cf162bc629b
- 출처 데이터셋
- uspto-grants-2010_02
- 특허 번호
- US07655689B2
반응 노트
불러오는 중…