2,4-Dichlorophenol → (2,4-Dichlorophenoxy)propanol

HRID 1654449ノート

反応式

HRID 1654449 の反応式
Br[CH2:2][CH2:3][CH2:4][OH:5].[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[OH:14].N12CCCN=C1CCCCC2>C(O)(C)C.C(Cl)Cl>[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[O:14][CH2:2][CH2:3][CH2:4][OH:5]

参加物

6

反応物 3

HCID 84492,4-DichlorophenolHCID 123083-Bromo-1-propanolHCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene

生成物 1

HCID 235019(2,4-Dichlorophenoxy)propanol収率 105.9%

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

A solution of 3-bromopropanol (53.86 g, 0.368 mol) in isopropanol is added dropwise to a mixture of 2,4-dichlorophenol (50 g, 0.307 mol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (70.05 g, 0.406 mol) in isopropanol at reflux. The reaction mixture is heated at reflux for 3 hours and concentrated in vacuo to obtain a residue. The residue is dissolved in methylene chloride and the organic solution is washed sequentially with 0.5N sodium hydroxide solution, 1M hydrochloric acid and brine, dried over MgSO4 and concentrated in vacuo to obtain an oil which solidifies to give the title product as a white solid (71.9 g, mp 53°-55° C.).

後処理

  1. temperatureat reflux
  2. temperatureThe reaction mixture is heated
  3. temperatureat reflux for 3 hours
  4. concentrationconcentrated in vacuo
  5. customto obtain a residue
  6. washthe organic solution is washed sequentially with 0.5N sodium hydroxide solution, 1M hydrochloric acid and brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo
  9. customto obtain an oil which

出典と根拠

ORDレコード
ord-44e71e535fee4b1088a7230e8a2bbd29
出典データセット
uspto-grants-1995_04
特許番号
US05407897

反応ノート

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