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Potassium Carbonate → 1-Bromo-2-methoxy-4-propoxybenzene

HRID 612613
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HRID 612613 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[O:9][CH3:10].C(=O)([O-])[O-].[K+].[K+].[CH2:17](I)[CH2:18][CH3:19]>CC(C)=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:17][CH2:18][CH3:19])=[CH:4][C:3]=1[O:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 3479554-Bromo-3-methoxyphenol

생성물 1

HCID 195949351-Bromo-2-methoxy-4-propoxybenzene수율 88%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Prepare a solution of 4-bromo-3-methoxyphenol (6.5 g, 32 mmole), and potassium carbonate (15 g) in acetone (250 mL) under argon. Add n-propyl iodide (9.0 g, 5.2 mL, 53 mmole) and heat to reflux overnight. Cool to room temperature and filter. Rotovap to condense and evaporate the solvents. Check by thin layer chromatagraphy (25% ethyl aceate/75% hexane). Wash three times with 100 mL 3% potassium hydroxide. Dry the organic layer with magnesium sulfate. Filter and rotovap. Purify by chromatography and place under high vacuum to obtain the title compound (6.9 g, 88%). Rf=0.60 (EtOAc/hexane; 25:75).

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후처리

  1. temperatureto reflux overnight
  2. filtrationfilter
  3. customRotovap to condense
  4. customevaporate the solvents
  5. washWash three times with 100 mL 3% potassium hydroxide
  6. dry with materialDry the organic layer with magnesium sulfate
  7. filtrationFilter
  8. customPurify by chromatography and place under high vacuum

출처 및 근거

ORD 기록
ord-c7076e5a361e4647a2e6332bb7696652
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06004959

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