1,2-Dibromoethane → 1,3-Dibromo-2-(2-bromoethoxy)benzene

HRID 603061

反応式

HRID 603061 の反応式
[Br:1][CH2:2][CH2:3]Br.[OH-].[Na+].[Br:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([Br:14])[C:9]=1[OH:15].C(OCC)(=O)C>O>[Br:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([Br:14])[C:9]=1[O:15][CH2:3][CH2:2][Br:1]

参加物

6

反応物 4

HCID 78391,2-DibromoethaneHCID 8857Ethyl AcetateHCID 118472,6-DibromophenolHCID 14798Sodium Hydroxide

生成物 1

HCID 292722841,3-Dibromo-2-(2-bromoethoxy)benzene収率 57%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1,2-Dibromoethane (5.0 ml, 58 mmol) was added to a solution of sodium hydroxide (2.5 g, 63 mmol) and 2,6-dibromophenol (14.5 g, 57.6 mmol) in 45 ml of water. The mixture was stirred under reflux for 20 hours and then extracted with ether. The combined organic layers was dried over Na2SO4, filtered and concentrated to give colorless oil. Silica gel chromatography, using a gradient of ethyl acetate, in hexanes to afforded 1,3-dibromo-2-(2-bromo-ethoxy)-benzene (11.55 g, 57% yield) as a colorless oil.

後処理

  1. temperatureunder reflux for 20 hours
  2. extractionextracted with ether
  3. dry with materialThe combined organic layers was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto give colorless oil

出典と根拠

ORDレコード
ord-e14deb98f14a49329f0a8cc62e38be85
出典データセット
uspto-grants-2011_03
特許番号
US07906648B2

関連ノート

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