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Dichloromethane → (4-Bromo-5-methylpyridin-2-yl)methanol

HRID 2080477
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2080477
FC(F)(F)C(O[C:6](=[O:11])[C:7](F)(F)F)=O.ClCCl.[Br:17][C:18]1[C:23]([CH3:24])=[CH:22][N+:21]([O-])=C(C)[CH:19]=1>CCCCCC>[Br:17][C:18]1[C:23]([CH3:24])=[CH:22][N:21]=[C:7]([CH2:6][OH:11])[CH:19]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 9845Trifluoroacetic anhydrideHCID 544438594-Bromo-2,5-dimethylpyridine 1-oxide

Produkt 1

HCID 23114663(4-Bromo-5-methylpyridin-2-yl)methanolAusbeute 83,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8058HexaneLösungsmittel

Versuchsvorschrift

Under an argon atmosphere, trifluoroacetic anhydride (20.6 ml, 0.146 mol) was added to a dichloromethane solution (100 ml) solution of 4-bromo-2,5-dimethylpyridine 1-oxide (9.8 g, 48.5 mmol) under ice cooling. The resulting mixture was stirred for 20 minutes and then, stirred at room temperature for 7.5 hours. The reaction mixture was concentrated under reduced pressure. To a dichloromethane solution (50 ml) of the residue was added a saturated aqueous solution (100 ml) of sodium bicarbonate. The resulting mixture was stirred for 14 hours. The reaction mixture was extracted with dichloromethane. The extract was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the hexane:ethyl acetate (=1:1) eluate was concentrated under reduced pressure to give the title compound (8.17 g, 40.4 mmol, 83%) as a yellow powder.

Aufarbeitung

  1. stirringstirred at room temperature for 7.5 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionTo a dichloromethane solution (50 ml) of the residue was added a saturated aqueous solution (100 ml) of sodium bicarbonate
  4. stirringThe resulting mixture was stirred for 14 hours
  5. extractionThe reaction mixture was extracted with dichloromethane
  6. dry with materialThe extract was dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue thus obtained
  9. concentrationethyl acetate (=1:1) eluate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-406bae1fc46848bb8fac4917346b95d2
Quelldatensatz
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07932271B2

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