Potassium Carbonate → 1-Ethynyl-3-(trifluoromethyl)benzene
反応式
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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-c30f806652554078a63ae90949880c26
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09439890B2
反応ノート
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