Ethyl Acetate → 4-(Difluoromethoxy)benzonitrile
反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1)#[N:2].Cl[C:11]([F:17])([F:16])C(OC)=O.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CN(C=O)C>[F:16][CH:11]([F:17])[O:9][C:6]1[CH:7]=[CH:8][C:3]([C:1]#[N:2])=[CH:4][CH:5]=1参加物
6
実験手順
4-Cyanophenol (0.12 G, 1.0 mmol, Aldrich), methyl chlorodifluoroacetate (0.29 g, 2.0 mmol, Aldrich) and potassium carbonate (0.29 g, 2.1 mmol) were combined in dry DMF (0.5 mL) under an argon atmosphere. After stirring at 75°-80° C. for 0.3 h, the mixture was cooled to RT, ethyl acetate (20 mL) was added and the organic layer was washed twice with 10% NaOH. The organic extract was dried (MgSO4), filtered and evaporated. The residue was purified by flash chromatography (silica gel, 20% ether/hexanes) to provide the title compound as a colorless solid (0.09 g, 53%). mp 34°-35° C.
後処理
- washthe organic layer was washed twice with 10% NaOH
- extractionThe organic extract
- dry with materialwas dried (MgSO4)
- filtrationfiltered
- customevaporated
- customThe residue was purified by flash chromatography (silica gel, 20% ether/hexanes)
出典と根拠
- ORDレコード
- ord-4972bb959a7b4018a8ed305bf737462c
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05731477
反応ノート
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