Sodium Hydroxide → HCID 59334623, Verbindung

HRID 1639740Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1639740
[N+:1]([C:4]1C=C([N+]([O-])=O)C=C[C:5]=1[O-])([O-])=O.[NH2:14][N+:15]1[CH:20]=[CH:19][CH:18]=[C:17]([CH2:21][OH:22])[CH:16]=1.[OH-].[Na+]>C(#N)C>[CH3:5][C:4]1[N:1]=[C:16]2[C:17]([CH2:21][OH:22])=[CH:18][CH:19]=[CH:20][N:15]2[N:14]=1

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 866419191-Amino-3-(hydroxymethyl)pyridinium 2,4-dinitrobenzenolate

Produkt 1

HCID 59334623HCID 59334623, VerbindungAusbeute 29 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of 1-amino-3-(hydroxymethyl)pyridinium 2,4-dinitrobenzenolate (100 g, 323 mmol) in acetonitrile (1.08 L), was added 2 N sodium hydroxide (485 mL) at room temperature, and the mixture was stirred for 12 hr. Acetonitrile was evaporated under reduced pressure, and the residual aqueous solution was extracted with 3 times with chloroform. The extract was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by recrystallization (ethyl acetate/hexane) to give the title compound (14.0 g, yield 29%).

Aufarbeitung

  1. customAcetonitrile was evaporated under reduced pressure
  2. extractionthe residual aqueous solution was extracted with 3 times with chloroform
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by recrystallization (ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-bdf46ed98c9c446f8c8f067321182f2f
Quelldatensatz
uspto-grants-2012_02
Patentnummer
US08110585B2

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