Ethanol → 5-Bromo-N-methyl-3-nitropyridin-2-amine

HRID 445621

Reaktionsgleichung

Reaktionsgleichung von HRID 445621
[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5](Cl)=[N:6][CH:7]=1.[CH3:12][NH2:13].CCO>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5]([NH:13][CH3:12])=[N:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 702EthanolHCID 6329MethylamineHCID 70194125-Bromo-2-chloro-3-nitropyridine

Produkt 1

HCID 108681495-Bromo-N-methyl-3-nitropyridin-2-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 5-bromo-2-chloro-3-nitropyridine (Matrix, Columbia, USA, 9.8 g, 41.3 mmol) in 250 ml THF was added 8 M methylamine in EtOH (Aldrich, Buchs, Switzerland, 12.9 ml, 103 mmol). The reaction mixture was stirred 1 h at rt then was quenched with 300 ml water. The precipite was filtered and the filtrate concentrated before being filtered again. The yellow solids were combined and dried to give the title compound as a yellow solid (HPLC: tR 3.13 min (Method A)).

Aufarbeitung

  1. customthen was quenched with 300 ml water
  2. filtrationThe precipite was filtered
  3. concentrationthe filtrate concentrated
  4. filtrationbefore being filtered again
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a355d5361bce4509af81f3ec9290f393
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08476294B2

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