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5-Bromo-4,6-dimethylpyridin-2-amine → HCID 178429301, Verbindung

HRID 1043890
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1043890
N[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([Br:9])=[C:4]([CH3:10])[N:3]=1.N([O-])=[O:12].[Na+]>S(=O)(=O)(O)O.O>[Br:9][C:5]1[C:6]([CH3:8])=[CH:7][C:2]([OH:12])=[N:3][C:4]=1[CH3:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 110308555-Bromo-4,6-dimethylpyridin-2-amineHCID 23668193Sodium Nitrite

Produkt 1

HCID 178429301HCID 178429301, VerbindungAusbeute 90,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

2-amino-5-bromo-4,6-dimethylpyridine (15 g) was dissolved in a mixed solution of sulfuric acid (14.2 mL) and water (212 mL). A solution of sodium nitrite (6.18 g) in water (31 mL) was added to the solution at 0° C. The reaction mixture was stirred at mom temperature for one hour, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate, and the desiccant was filtered off. The filtrate was concentrated under reduced pressure. MTBE was added to the residue to precipitate the solid, followed by filtration. The filtration residue was washed with MTBE to give the title compound (13.7 g).

Aufarbeitung

  1. extractionfollowed by extraction with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationthe desiccant was filtered off
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. additionMTBE was added to the residue
  6. customto precipitate the solid
  7. filtrationfollowed by filtration
  8. washThe filtration residue was washed with MTBE

Quellen und Nachweise

ORD-Eintrag
ord-a776de9b47cf4981b1071060197f4f51
Quelldatensatz
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08563565B2

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