反応式
[Na].[I:2][C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.Cl[CH2:11][CH2:12][OH:13].[Cl-].[NH4+]>C(O)C>[I:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH2:11][CH2:12][OH:13])=[CH:5][CH:4]=1参加物
6
実験手順
Sodium (0.53 g) was dissolved in ethanol (50 ml) under nitrogen and 4-iodophenol (5.0 g), and 2-chloroethanol (3.93 g), were added successively. The mixture was refluxed for 18 h, treated with saturated aqueous ammonium chloride (50 ml) and evaporated. The aqueous residue was extracted with ER (3×100 ml) and the dried extract was evaporated onto silica (Merck 9385; 50 ml) and purified by [C] eluted with cyclohexane-ER (7:3) followed by cyclohexane-ER (1:1) to give the title compound (3.0 g) m.p. 76°-77°.
後処理
- temperatureThe mixture was refluxed for 18 h
- customevaporated
- extractionThe aqueous residue was extracted with ER (3×100 ml)
- extractionthe dried extract
- customwas evaporated onto silica (Merck 9385; 50 ml)
- custompurified by [C]
- washeluted with cyclohexane-ER (7:3)
出典と根拠
- ORDレコード
- ord-bb88b4021fb443c68845c639338c7086
- 出典データセット
- uspto-grants-1991_02
- 特許番号
- US04990505
関連ノート
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