Diethyl Ether → HCID 22063668, Verbindung

HRID 1828542

Reaktionsgleichung

Reaktionsgleichung von HRID 1828542
[NH2:1][C:2]1[C:3]([CH3:12])=[CH:4][C:5]([NH:8][C:9](=[O:11])[CH3:10])=[N:6][CH:7]=1.[N:13]([O-])=O.[Na+].C(OCC)C.[F:22][B-:23]([F:26])([F:25])[F:24].[H+]>>[F:22][B-:23]([F:26])([F:25])[F:24].[C:9]([NH:8][C:5]1[N:6]=[CH:7][C:2]([N+:1]#[N:13])=[C:3]([CH3:12])[CH:4]=1)(=[O:11])[CH3:10]

Komponenten

5

Edukt 4

HCID 3283Diethyl EtherHCID 28118Tetrafluoroboric acidHCID 22063573N-(5-Amino-4-methylpyridin-2-yl)acetamide2×HCID 23668193Sodium Nitrite

Produkt 1

HCID 22063668HCID 22063668, Verbindung

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

The N1-(5-amino-4-methyl-2-pyridyl)acetamide (8.00 g, 48.4 mmol) obtained in (B) was dissolved in tetrafluoroboric acid (160 ml) and slowly added dropwise with an aqueous solution (40 ml) of sodium nitrite (3.51 g, 50.8 mmol) at −20° C. under nitrogen atmosphere. The reaction mixture was further stirred at −10° C. for 1 hour and added with diethyl ether (800 ml), and the deposited white solid was collected by filtration and washed with diethyl ether to obtain the title compound (14.7 g, quantitative).

Aufarbeitung

  1. filtrationthe deposited white solid was collected by filtration
  2. washwashed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-cbb21bec42474f60a019da7ee26d175a
Quelldatensatz
uspto-grants-2006_06
Patentnummer
US07056917B2

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