反応式
[I:1]N1C(=O)CCC1=O.[F:9][C:10]([F:20])([F:19])[O:11][C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1.S(=O)(=O)(O)O>C(O)(=O)C.O>[I:1][C:14]1[CH:13]=[C:12]([O:11][C:10]([F:19])([F:20])[F:9])[CH:17]=[CH:16][C:15]=1[OH:18]参加物
実験手順
To a suspension of N-iodosuccinimide (6.95 g, 31 mmol) in glacial acetic acid (2 ml) was added 4-trifluoromethoxy phenol (4.0 ml, 31 mmol) and, after 5 minutes, concentrated sulphuric acid (0.5 ml, 9 mmol). The pale brown suspension was stirred at room temperature under nitrogen for 48 hours before diluting with water and extracting with dichloromethane. Organic extract was washed with water, saturated aqueous sodium thiosulphate solution, water, dried over magnesium sulfate and decolourising charcoal added. The resulting suspension was left to stand for 30 minutes before filtering through a short pad of silica gel eluting with dichloromethane. The solvent was evaporated in vacuo to give the title compound as an oil, 8.78 g, 94% yield.
後処理
- extractionextracting with dichloromethane
- extractionOrganic extract
- washwas washed with water, saturated aqueous sodium thiosulphate solution, water
- dry with materialdried over magnesium sulfate
- additionadded
- waitThe resulting suspension was left
- waitto stand for 30 minutes
- filtrationbefore filtering through a short pad of silica gel eluting with dichloromethane
- customThe solvent was evaporated in vacuo
出典と根拠
- ORDレコード
- ord-ed5b836a8b304d37a4e16c36dca41b8e
- 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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