Hydrochloric Acid → 6-Methoxy-4-methylpyridin-3-amine

HRID 53529

Reaktionsgleichung

Reaktionsgleichung von HRID 53529
Cl.[CH3:2][O:3][C:4]1[CH:9]=[C:8]([CH3:10])[C:7]([N+:11]([O-])=O)=[CH:6][N:5]=1>C(O)(=O)C>[NH2:11][C:7]1[C:8]([CH3:10])=[CH:9][C:4]([O:3][CH3:2])=[N:5][CH:6]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 2431692-Methoxy-4-methyl-5-nitropyridine

Produkt 1

HCID 2431706-Methoxy-4-methylpyridin-3-amineAusbeute 93,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A mixture of stannous chloride dihydrate (41 g) and concentrated hydrochloric acid (40 ml) was added slowly to a solution of 2-methoxy-4-methyl-5-nitropyridine (5.1 g) in acetic acid (40 ml), maintaining the temperature below 35° C. The resulting mixture was stirred at room temperature for 2 hours, and then allowed to stand overnight in the refrigerator. The solid was collected and both solid and supernatant were separately basified with a 20% sodium hydroxide solution. The product was extracted with chloroform, combined, dried (anhydrous magnesium sulfate) and concentrated to give 3.9 g of the title compound as a solid, suitable for use in the next reaction.

Aufarbeitung

  1. temperaturemaintaining the temperature below 35° C
  2. waitto stand overnight in the refrigerator
  3. customThe solid was collected
  4. extractionThe product was extracted with chloroform
  5. dry with materialdried (anhydrous magnesium sulfate)
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-da1bc058a21e4a1093907d85c422255a
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05620974

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