Potassium Hydroxide → HCID 18182294, Verbindung

HRID 1359266

Reaktionsgleichung

Reaktionsgleichung von HRID 1359266
[Br:1]Br.[Br-].[K+].[CH2:5]([C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[N:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[OH-].[K+].S([O-])([O-])=O.[Na+].[Na+]>[Cl-].[NH4+].[NH4+].[NH4+].[NH4+].[Cl-].[Cl-].[Cl-].O>[CH2:5]([CH:12]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[N:13]1[Br:1])[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1

Komponenten

8

Edukt 5

HCID 14797Potassium HydroxideHCID 24408BromineHCID 24437Sodium SulfiteHCID 253877Potassium Bromide2×HCID 219422742-Benzyl-6-methoxypyridine

Produkt 1

HCID 18182294HCID 18182294, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 22266888HCID 22266888, VerbindungKatalysatorHCID 962WaterLösungsmittel2×

Versuchsvorschrift

A mixed solution of 17 ml of bromine, 90 g of potassium bromide and 450 ml of water was added dropwise into a mixture of 60 g of 2-benzyl-6-methoxypyridine (Production Example 2-b), 90 g of potassium bromide, 450 ml of water, 20 g of potassium hydroxide and 2.5 g of tetraammonium chloride over 2 hours under stirring in an ice bath. After stirring overnight as it was, sodium sulfite was added thereto and the mixture was extracted with hexane. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was subjected to silica gel column chromatography to elute with 0.5-1.5% of ethyl acetate/hexane, to give 72.5 g of the target compound.

Aufarbeitung

  1. stirringAfter stirring overnight as it
  2. extractionthe mixture was extracted with hexane
  3. washThe organic phase was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was removed
  6. washto elute with 0.5-1.5% of ethyl acetate/hexane

Quellen und Nachweise

ORD-Eintrag
ord-0314bc1e8d6b4fe0a3167db30808daec
Quelldatensatz
uspto-grants-2003_07
Patentnummer
US06599917B1

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