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

HRID 1668746
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HRID 1668746 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 536995421,3-Dibromo-5-ethoxybenzene

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6569Methyl Ethyl Ketone용매

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이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트
온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e8ad1ba1c21a4873b750436bb00270fe
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989449B2

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