2-Phenylpyridine → 2-Phenylpyridine 1-Oxide

HRID 418051

Reaktionsgleichung

Reaktionsgleichung von HRID 418051
ClC1C=CC=C(C(OO)=[O:9])C=1.[C:12]1([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C([O-])(O)=O.[Na+]>C(Cl)Cl>[C:12]1([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][N+:19]=2[O-:9])[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

Komponenten

5

Edukt 3

HCID 138872-PhenylpyridineHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium Bicarbonate

Produkt 1

HCID 3024892-Phenylpyridine 1-OxideAusbeute 79,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

3-chloroperbenzoic acid (19 g) was added portionwise to an ice-cold solution of 2-phenylpyridine (10 g) in DCM (30 ml). The mixture was allowed to warm to RT and was stirred at RT for 4 h. 100 ml of a NaHCO3 solution were added to the reaction mixture and the phases were separated. The aq. phase was further extracted with DCM and the combined org. phases were washed with an aq. NaHSO3 (40%) solution and evaporated off. Recrystallisation (EA) afforded 8.77 g of the desired compound.

Aufarbeitung

  1. customthe phases were separated
  2. extractionThe aq. phase was further extracted with DCM
  3. washphases were washed with an aq. NaHSO3 (40%) solution
  4. customevaporated off
  5. customRecrystallisation (EA)

Quellen und Nachweise

ORD-Eintrag
ord-a44663e670ec4b0d82d1353224ea7e0e
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08093250B2

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