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Diethyl Sulfate → 1,3-Dibromo-5-ethoxybenzene

HRID 1668746
ノート
印刷プレビュー

反応式

HRID 1668746 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([Br:8])[CH:7]=1.C(=O)([O-])[O-].[K+].[K+].S(OCC)(O[CH2:20][CH3:21])(=O)=O>CC(=O)CC.ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([O:9][CH2:20][CH3:21])[CH:5]=[C:6]([Br:8])[CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6163Diethyl SulfateHCID 11430Potassium CarbonateHCID 122803,5-Dibromophenol

生成物 1

HCID 536995421,3-Dibromo-5-ethoxybenzene

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6569Methyl Ethyl Ketone溶媒

反応条件

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート
温度
90 °C

実験手順

A dispersion of 3,5-dibromophenol (0.398 g, 1.6 mmol) and potassium carbonate (0.437 g, 3.2 mmol) in 2-butanone (4 mL) was treated with diethyl sulfate (0.246 g, 1.6 mmol) and the reaction mixture heated at 90° C. for 15 hours. The resulting thick suspension was cooled to room temperature, diluted with dichloromethane and extracted with water. The organic layer was separated, dried over sodium sulfate and evaporated under reduced pressure. The title compound was obtained as a light brown oil (0.38 g, 86% of theory) which was used in the next step without further purification.

後処理

  1. temperatureThe resulting thick suspension was cooled to room temperature
  2. extractionextracted with water
  3. customThe organic layer was separated
  4. dry with materialdried over sodium sulfate
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-e8ad1ba1c21a4873b750436bb00270fe
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07989449B2

反応ノート

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