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Phenol → 2-Bromo-5-phenoxypyridine

HRID 897455
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 897455
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[Br:10][C:11]1[CH:16]=[C:15](Br)[CH:14]=[CH:13][N:12]=1>CN(C)C=O>[Br:10][C:11]1[CH:16]=[CH:15][C:14]([O:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:13][N:12]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 996PhenolHCID 24758Sodium hydrideHCID 8171042,4-Dibromopyridine

Produkt 1

HCID 223469212-Bromo-5-phenoxypyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of phenol (1.99 g, 0.021 mol) in N,N-dimethylformamide (60 mL) was cooled to 0° C. and a 60% suspension of sodium hydride in parafine (0.89 g, 0.022 mol) was added at once. The mixture was stirred at this temperature for 10 min and 2,4-dibromopyridine was added at once. The mixture was allowed to warm up to ambient temperature while stirring under nitrogen for 72 hours and heated at 70° C. for 24 hours. The solvent was removed under reduced pressure; the residue was dissolved in ethyl acetate (150 mL) and washed with saturated aqueous sodium bicarbonate solution (100 mL), brine (80 mL), dried with magnesium sulfate and evaporated. The residue was purified by preparative RP-LC/MS (Gilson-Micromass C18, 5 m, 130 A, 21 cm, 0%-100% acetonitrile-0.1M ammonium acetate over 9 min, 25 mL/min) to give 2-bromo-5-phenoxypyridine as a yellow oil (1.40 g, 0.0056 mol): 1H NMR (DMSO-d6, 400 MHz) 8.28 (s, 1H), 8.07 (d, 1H), 7.45 (t, 2H), 7.25 (t, 1H), 7.16 (d, 2H), 7.04 (d, 1H); MS: MH+ 250.

Aufarbeitung

  1. stirringwhile stirring under nitrogen for 72 hours
  2. temperatureheated at 70° C. for 24 hours
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate (150 mL)
  5. washwashed with saturated aqueous sodium bicarbonate solution (100 mL), brine (80 mL)
  6. dry with materialdried with magnesium sulfate
  7. customevaporated
  8. customThe residue was purified by preparative RP-LC/MS (Gilson-Micromass C18, 5 m, 130 A, 21 cm, 0%-100% acetonitrile-0.1M ammonium acetate over 9 min, 25 mL/min)

Quellen und Nachweise

ORD-Eintrag
ord-8cddeabc352448e98ebab835deb3b4da
Quelldatensatz
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06921763B2

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