反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]#[N:10])[CH:5]=[CH:6][CH:7]=1.[CH2:11](Br)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[CH2:11]([O:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]#[N:10])[CH:5]=[CH:6][CH:7]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1参加物
反応条件
- 温度
- 90 °C
実験手順
3-Hydroxyphenylacetonitrile (834 mg, 6.26 mmol) was dissolved in DMF (10 ml), and to this solution were successively added benzyl bromide (0.82 ml, 6.89 mmol, 1.1 eq) and anhydrous potassium carbonate (1.30 g, 9.40 mmol, 1.5 eq). The mixture was stirred under heating at 90° C. for 1.5 hours. This reaction mixture was cooled to room temperature, and water (20 ml) was added. The mixture was extracted twice with ethyl acetate (40 ml). The organic layers were combined, washed with saturated brine (80 ml) and dried over anhydrous sodium sulfate. The drying agent was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by column chromatography (hexane/ethyl acetate=1/1) to give (3-benzyloxyphenyl)acetonitrile (1.21 g, 86.8%).
後処理
- temperatureThis reaction mixture was cooled to room temperature
- extractionThe mixture was extracted twice with ethyl acetate (40 ml)
- washwashed with saturated brine (80 ml)
- dry with materialdried over anhydrous sodium sulfate
- filtrationThe drying agent was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- customThe obtained residue was purified by column chromatography (hexane/ethyl acetate=1/1)
出典と根拠
- ORDレコード
- ord-014b240ba2084d1681e8d47222a0e1e9
- 出典データセット
- uspto-grants-2000_01
- 特許番号
- US06017919
関連ノート
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