Potassium Carbonate → 1-Ethynyl-3-(trifluoromethyl)benzene
반응식
C[Si](C)(C)[C:3]#[C:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([F:14])([F:13])[F:12])[CH:6]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[C:4]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([F:12])([F:13])[F:14])[CH:6]=1)#[CH:3]참가 물질
4
실험 절차
To a solution of trimethyl((3-(trifluoromethyl)phenyl)ethynyl)silane (0.500 g, 2.06 mmol) in ethanol (10 mL) was added potassium carbonate (0.253 g, 1.8 mmol) and the reaction mixture was stirred at RT for 18 h. The reaction mass was quenched in water, neutralized with dil. HCl and extracted with hexane and concentrated to afford 0.200 g of the crude product which was further purified by column chromatography using silica (60-120 mesh) eluting with pet. ether to afford 0.500 g of pure product. 1H NMR (300 MHz, DMSO d6): δ 4.41 (s, 1H), 7.64 (d, J=7.5 Hz, 1H), 7.77-7.81 (m, 3H).
후처리
- customThe reaction mass was quenched in water
- extractionextracted with hexane
- concentrationconcentrated
- customto afford 0.200 g of the crude product which
- customwas further purified by column chromatography
- washeluting with pet. ether
출처 및 근거
- ORD 기록
- ord-d9c25503165c4bbf86de75c231c59820
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09096545B2
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