2-Amino-3,4-diethoxycarbonyl-6-phenylpyridine hydrochloride → 3,4-Diethoxycarbonyl-6-phenyl-2-pyridone

HRID 37466Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 37466
Cl.N[C:3]1[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:6]=[C:5]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[N:4]=1.N([O-])=[O:26].[Na+]>Cl.O1CCOCC1.O>[CH2:12]([O:11][C:9]([C:8]1[C:3](=[O:26])[NH:4][C:5]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:6][C:7]=1[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:10])[CH3:13]

Komponenten

6

Edukt 2

HCID 199356132-Amino-3,4-diethoxycarbonyl-6-phenylpyridine hydrochlorideHCID 23668193Sodium Nitrite

Produkt 1

HCID 199356223,4-Diethoxycarbonyl-6-phenyl-2-pyridone

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 313Hydrochloric AcidLösungsmittelHCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

In a mixture of 90 ml of 2% hydrochloric acid and 60 ml of dioxane was dissolved 3.50 g (10 mmol) of 2-amino-3,4-diethoxycarbonyl-6-phenylpyridine hydrochloride. A solution of 0.83 g (1.2 eq.) of sodium nitrite dissolved in 3 ml of water was added dropwise thereto. The mixture was stirred at room temperature for 4 hours and left standing overnight. The solvent was distilled off. The resulting crystals were collected by filtration with water. The crystals were recrystallized from ethanol, to give pale yellow prisms.

Aufarbeitung

  1. additionwas added dropwise
  2. waitleft
  3. waitstanding overnight
  4. distillationThe solvent was distilled off
  5. filtrationThe resulting crystals were collected by filtration with water
  6. customThe crystals were recrystallized from ethanol
  7. customto give pale yellow prisms

Quellen und Nachweise

ORD-Eintrag
ord-3ba45d3f0a9040be8c9e7621a06f83d8
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05420275

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