2-Chloroethanol → 2-(4-Iodophenoxy)ethanol

HRID 981145

反応式

HRID 981145 の反応式
[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

  1. temperatureThe mixture was refluxed for 18 h
  2. customevaporated
  3. extractionThe aqueous residue was extracted with ER (3×100 ml)
  4. extractionthe dried extract
  5. customwas evaporated onto silica (Merck 9385; 50 ml)
  6. custompurified by [C]
  7. 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

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