Pyridine → HCID 19935586, Verbindung

HRID 37500

Reaktionsgleichung

Reaktionsgleichung von HRID 37500
Cl[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:5]([N+:18]([O-:20])=[O:19])=[C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[N:3]=1.[NH:27]1[CH:31]=[N:30][CH:29]=[N:28]1.N1C=CC=CC=1>ClCCCl>[CH2:11]([O:10][C:8]([C:7]1[C:2]([N:27]2[CH:31]=[N:30][CH:29]=[N:28]2)=[N:3][C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:5]([N+:18]([O-:20])=[O:19])[C:6]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:9])[CH3:12]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 92571H-1,2,4-TriazoleHCID 199355872-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine

Produkt 1

HCID 19935586HCID 19935586, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 111,2-DichloroethaneLösungsmittel

Versuchsvorschrift

A mixture of 0.379 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, 0.2 g of (1H-1,2,4-triazole, 0.2 ml of pyridine and 15 ml of 1,2-dichloroethane was reacted at 80° C. for 18 hours. After the reaction mixture was concentrated, the concentrate was extracted with ethyl acetate. The extract was washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate. After the solvent was distilled off, the residue was subjected to silica gel column chromatography (eluent:dichloromethane/ethyl acetate 4:1), to give 0.19 g of the title compound as yellow crystals.

Aufarbeitung

  1. customwas reacted at 80° C. for 18 hours
  2. concentrationAfter the reaction mixture was concentrated
  3. extractionthe concentrate was extracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materiala saturated aqueous solution of sodium chloride and dried over sodium sulfate
  6. distillationAfter the solvent was distilled off

Quellen und Nachweise

ORD-Eintrag
ord-fe046a86aab84ef0b6811df7ef1c1e4c
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05420275

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