反応式
[I:1]N1C(=O)CCC1=O.[F:9][C:10]([F:19])([F:18])[C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][CH:12]=1.S(=O)(=O)(O)O>C(O)(=O)C.O>[I:1][C:13]1[CH:12]=[C:11]([C:10]([F:18])([F:19])[F:9])[CH:16]=[CH:15][C:14]=1[OH:17]参加物
実験手順
To a suspension of N-iodosuccinimide (11.10 g, 49.5 mmol) in glacial acetic acid (40 ml) was added 4-trifluoromethyl phenol (8.02 g, 49.5 mmol) and, after 5 minutes, concentrated sulphuric acid (0.87 ml, 14.8 mmol). The pale brown/red suspension was stirred at room temperature under nitrogen for 48 hours before diluting with water and extracting with dichloromethane. The organic extract was washed with water, saturated aqueous sodium thiosulphate solution, water, dried over magnesium sulphate before decolourising charcoal added. The suspension was left to stand for 10 minutes before filtering through a short pad of silica gel eluting with dichloromethane. The solvent was evaporated in vacuo to give an oil which was purified by flash column chromatography on silica eluting with dichloromethane to give the title compound as a pale yellow oil, 9.017 g, 63% yield.
後処理
- extractionextracting with dichloromethane
- extractionThe organic extract
- washwas washed with water, saturated aqueous sodium thiosulphate solution, water
- dry with materialdried over magnesium sulphate
- additionadded
- waitThe suspension was left
- waitto stand for 10 minutes
- filtrationbefore filtering through a short pad of silica gel eluting with dichloromethane
- customThe solvent was evaporated in vacuo
- customto give an oil which
- customwas purified by flash column chromatography on silica eluting with dichloromethane
出典と根拠
- ORDレコード
- ord-63a64ba6d2f3459284dce01856af67e8
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541588B2
関連ノート
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