반응식
[Br:1][C:2]1[C:3](I)=[C:4]([CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1)[NH2:5].[C:14]([Si:16]([CH3:19])([CH3:18])[CH3:17])#[CH:15]>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu]I.C(N(CC)CC)C>[Br:1][C:2]1[C:3]([C:15]#[C:14][Si:16]([CH3:19])([CH3:18])[CH3:17])=[C:4]([CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1)[NH2:5]참가 물질
6
반응물 2
생성물 1
시약·촉매·용매 3
반응 조건
- 온도
- 80 °C
실험 절차
A mixture of 3-bromo-2-iodo-5-(trifluoromethyl)aniline (5.21 g), ethynyl(trimethyl)silane (2.21 mL), triethylamine (100 mL), dichlorobis(triphenylphosphine)palladium(II) (1.00 g) and copper(I) iodide (0.271 g) was stirred overnight at 80° C. under nitrogen atmosphere. The solvent was evaporated under reduced pressure, to the residue was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.70 g).
후처리
- customThe solvent was evaporated under reduced pressure, to the residue
- additionwas added saturated aqueous ammonium chloride solution
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
출처 및 근거
- ORD 기록
- ord-c3d634ed7fb94bde88394e1c8c988508
- 출처 데이터셋
- uspto-grants-2016_03
- 특허 번호
- US09296746B2
연결된 노트
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