Hydrochloric Acid → 3-Fluoro-2-hydroxymethyl-6-methoxyphenol
反応式
[F:1][C:2]1[C:7]([CH:8]=[O:9])=[C:6]([OH:10])[C:5]([O:11][CH3:12])=[CH:4][CH:3]=1.C1COCC1.[BH4-].[Na+].Cl>C(O)C>[F:1][C:2]1[C:7]([CH2:8][OH:9])=[C:6]([OH:10])[C:5]([O:11][CH3:12])=[CH:4][CH:3]=1参加物
6
実験手順
To a solution of 6.85 g of 6-fluoro-2-hydroxy-3-methoxybenzaldehyde [CAS No. 457628-15-8] in 200 ml of an ethanol:THF=1:1 mixed solvent there was added 1.52 g of sodium borohydride while cooling on ice. After stirring at room temperature for 30 minutes, 1N hydrochloric acid was added to the reaction mixture while cooling on ice. The organic layer was extracted with ethyl acetate and dried over anhydrous magnesium sulfate. The desiccating agent was filtered off, and the filtrate was concentrated under reduced pressure to give 3-fluoro-2-hydroxymethyl-6-methoxyphenol (6.1 g, crude product).
後処理
- temperaturewhile cooling on ice
- temperaturewhile cooling on ice
- extractionThe organic layer was extracted with ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- filtrationThe desiccating agent was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-dfb9de0178964e7d93275054fc0d0bb5
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08163787B2
反応ノート
読み込み中…