Chloroacetonitrile → 3-Fluorophenoxyacetonitrile
反応式
[F:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:16][C:17]#[N:18]>CN(C=O)C.CCOC(C)=O>[F:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][CH2:16][C:17]#[N:18]参加物
6
反応条件
- 温度
- 50 °C
実験手順
To a solution of 3-fluorophenol (560 mg, 5.0 mmol) in DMF (10 mL) is added potassium carbonate (828 mg, 6.0 mmol) followed by chloroacetonitrile (0.315 mL, 50.0 mmol). The reaction mixture is stirred and heated at 50° C. for 14 h. The reaction mixture is cooled to RT, diluted with EtOAc, and washed with water, brine, then dried (MgSO4), and filtered. The filtrate is evaporated, and the residue purified by chromatography on silica gel; elution with dichloromethane gives 712 mg of the product 386.
後処理
- temperatureThe reaction mixture is cooled to RT
- washwashed with water, brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- customThe filtrate is evaporated
- customthe residue purified by chromatography on silica gel
- washelution with dichloromethane
出典と根拠
- ORDレコード
- ord-679042b22ecb452c904ab20fb5acda8e
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741493B2
反応ノート
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