Triethylamine → HCID 178502659, Verbindung

HRID 2187235Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2187235
CS[C:3]([NH:8][CH2:9][C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)=[CH:4][N+:5]([O-:7])=[O:6].[CH3:16][O:17][NH3+:18].[Cl-].C(N(CC)CC)C>C(O)C(C)C>[CH3:16][O:17][N:18]=[C:3]([NH:8][CH2:9][C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)[CH2:4][N+:5]([O-:7])=[O:6]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 11639O-methylhydroxylammonium chlorideHCID 70155832HCID 70155832, Verbindung

Produkt 1

HCID 178502659HCID 178502659, VerbindungAusbeute 31,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6560IsobutanolLösungsmittel2×

Versuchsvorschrift

To 3 ml of isobutyl alcohol was added 0.75 g (0.0033 mole) of 1-methylthio-1-(3-pyridylmethyl)amino-2-nitroethylene, followed by addition of 0.56 g of 0-methylhydroxylamine hydrochloride at 100-110° C. Then, a solution of 0.93 ml of triethylamine in 1 ml of isobutyl alcohol was added dropwise at the same temperature with stirring over a period of 30 minutes. After completion of dropwise addition, the reaction mixture was allowed to cool to room temperature and the solvent was distilled off. The residue was purified by silica gel column chromatography [eluents: MeOH—CHCl3 (1:3) in the first run and MeOH—CHCl3 (1:10) in the second run] to give 0.23 g of the title compound as yellow crystals.

Aufarbeitung

  1. additionAfter completion of dropwise addition
  2. distillationthe solvent was distilled off
  3. customThe residue was purified by silica gel column chromatography [eluents

Quellen und Nachweise

ORD-Eintrag
ord-8471605050ac46ec9b29b3d11b907ee3
Quelldatensatz
uspto-grants-2002_06
Patentnummer
US06407248B1

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