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Hydrochloric Acid → 3-Methyl-6-hydroxybenzofuran

HRID 1107864
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인쇄 미리보기

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HRID 1107864 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[O:5][CH2:6][C:7](=O)[CH3:8].[OH-].[K+].Cl>>[CH3:8][C:7]1[C:10]2[CH:11]=[CH:12][C:2]([OH:1])=[CH:3][C:4]=2[O:5][CH:6]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 18786125(3-Hydroxyphenoxy)acetone

생성물 1

HCID 108556243-Methyl-6-hydroxybenzofuran수율 60.4%

반응 조건

온도
5 °C

실험 절차

3 g (18 mmol) of (3-hydroxyphenoxy)acetone and 400 ml of a 0.1M potassium hydroxide solution are introduced into a 1 l three-necked flask equipped with a reflux condenser. Heating is carried out at reflux for 6 hours. The reaction mixture is cooled to 5° C., a molar hydrochloric acid solution is added, in order to obtain a pH of approximately 5, and extraction is carried out with ethyl ether (3×150 ml). The organic phases are combined, dried over magnesium sulphate and concentrated. The residue is purified by silica column chromatography (elution solvent: 8/2 cyclohexane/ethyl acetate). 1.61 g of 3-methyl-6-hydroxybenzofuran are obtained--M.p.: 92° C.

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후처리

  1. customequipped with a reflux condenser
  2. temperatureHeating
  3. temperatureat reflux for 6 hours
  4. customto obtain
  5. extractiona pH of approximately 5, and extraction
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated
  8. customThe residue is purified by silica column chromatography (elution solvent: 8/2 cyclohexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-80cae4e0f7424c6ea2f4512a170fc7a7
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06063810

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