反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Br:8])[C:3]=1[OH:9].C(=O)([O-])[O-].[K+].[K+].Br[CH2:17][CH2:18][Cl:19]>CN(C=O)C>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Br:8])[C:3]=1[O:9][CH2:17][CH2:18][Cl:19]参加物
5
実験手順
A solution comprising 2,6-dibromophenol (3.90 g, 15.00 mmol), potassium carbonate (2.48 g, 17.94 mmol) and DMF (40 ml) was added with 1-bromo-2-chloro ethane (4.30 g, 29.98 mmol) and stirred at room temperature for 16 hours. The reaction solution was concentrated and liquid separation was carried out with ethyl acetate-water. The organic layer was washed with saturated sodium chloride water and dried with anhydrous sodium sulfate. The residue obtained by concentration was purified by silica gel column chromatography (n-hexane) to obtain the target compound (4.75 g, quant.) as a colorless oily substance.
後処理
- concentrationThe reaction solution was concentrated
- customliquid separation
- washThe organic layer was washed with saturated sodium chloride water
- dry with materialdried with anhydrous sodium sulfate
- customThe residue obtained by concentration
- customwas purified by silica gel column chromatography (n-hexane)
- customto obtain the target compound (4.75 g, quant.) as a colorless oily substance
出典と根拠
- ORDレコード
- ord-9b0bbbb9ec794185867fefed5ca2f758
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07951799B2
関連ノート
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