Bromine → 1-(5-Bromo-3-(trifluoromethyl)pyridin-2-yl)ethanol
反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[C:4]([CH:9]([OH:11])[CH3:10])=[N:5][CH:6]=[CH:7][CH:8]=1.[Br:14]Br>CO>[Br:14][C:7]1[CH:8]=[C:3]([C:2]([F:1])([F:12])[F:13])[C:4]([CH:9]([OH:11])[CH3:10])=[N:5][CH:6]=1参加物
4
実験手順
Dissolve 1-(3-(trifluoromethyl)pyridin-2-yl)ethanol (8.8 g, 0.046 moles) in anhydrous MeOH (80 mL) and add bromine (2.35 mL) dropwise at room temperature. Reflux the mixture under N2 atmosphere for 3 weeks with the addition of bromine (1.0 mL) on each day. Concentrate the reaction mixture under vacuum, dilute with water (100 mL), neutralize with NaHCO3, extract with EtOAc (3×100 mL) and dry (MgSO4). Filter the dried extract and concentrate under vacuum to afford a yellow oil. Purify the crude product by column chromatography to afford the title compound as a pale yellow oil.
後処理
- temperatureReflux the mixture under N2 atmosphere for 3 weeks
- concentrationConcentrate the reaction mixture under vacuum
- additiondilute with water (100 mL)
- extractionextract with EtOAc (3×100 mL)
- dry with materialdry (MgSO4)
- filtrationFilter the dried
- extractionextract
- concentrationconcentrate under vacuum
- customto afford a yellow oil
- customPurify the crude product by column chromatography
出典と根拠
- ORDレコード
- ord-5570b20951ca44dfbb6b189522bad0a0
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07935702B2
反応ノート
読み込み中…