Sodium Hydroxide → 2-Amino-3-bromo-6-methylpyridine

HRID 2294887Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2294887
[NH2:1][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[CH:4][CH:3]=1.[Br:9]Br.[OH-].[Na+]>S(=O)(=O)(O)O.O>[NH2:1][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[Br:9]

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 157652-Amino-6-methylpyridineHCID 24408Bromine

Produkt 1

HCID 27344162-Amino-3-bromo-6-methylpyridineAusbeute 55,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

32.4 g (0.3 mole) of 6-aminopicoline was dissolved in a mixture of 28 g of conc. sulfuric acid and 120 ml of water and the resulting solution was cooled in ice water. 52.8 g (0.33 mole) of bromine was added dropwise to the solution over 30 minutes at 0° C. The reaction solution was stirred for 20 minutes at room temperature and neutralized with cold aqueous NaOH solution. The resultant was filtered and the solid was purified with column chromatography using methylene chloride and ethyl acetate as an eluent to obtain 31 g of the title compound (yield 55%).

Aufarbeitung

  1. filtrationThe resultant was filtered
  2. customthe solid was purified with column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-3937fc1e153a4492b650464d69a4578b
Quelldatensatz
uspto-grants-1997_11
Patentnummer
US05691348

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