Ethanol → Ethyl 6-amino-5-nitropyridine-3-carboxylate

HRID 1644586Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1644586
[NH2:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1.S(=O)(=O)(O)O.[CH2:19](O)[CH3:20]>>[NH2:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]([C:6]([O:8][CH2:19][CH3:20])=[O:7])=[CH:4][N:3]=1

Komponenten

4

Versuchsvorschrift

A solution of 6-amino-5-nitronicotinic acid (10 g) and concentrated sulfuric acid (20 ml) in ethanol (250 ml) was heated under reflux for 18 hr. The reaction mixture was concentrated, diluted with water and adjusted with sodium hydrogencarbonate to pH 8. The precipitated crystals were collected by filtration and washed with water to give the title compound (8.5 g, yield 73%) as yellow crystals. purity 84%. M+H: 212.

Aufarbeitung

  1. temperatureunder reflux for 18 hr
  2. concentrationThe reaction mixture was concentrated
  3. additiondiluted with water
  4. filtrationThe precipitated crystals were collected by filtration
  5. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-0a933b6db7ba42edaa12b86b107ed684
Quelldatensatz
uspto-grants-2012_02
Patentnummer
US08124617B2

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