4-Aminopyridine → HCID 59427333, Verbindung

HRID 1013705Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1013705
[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[CH2:5][C:4](=[O:9])[O:3]1.[CH:11](OCC)(OCC)OCC.[N:21]1[CH:26]=[CH:25][C:24]([NH2:27])=[CH:23][CH:22]=1>CCCCCC>[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[C:5](=[CH:11][NH:27][C:24]2[CH:25]=[CH:26][N:21]=[CH:22][CH:23]=2)[C:4](=[O:9])[O:3]1

Komponenten

5

Edukt 3

HCID 17274-AminopyridineHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 31214Ethyl orthoformate

Produkt 1

HCID 59427333HCID 59427333, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8058HexaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

In a dried 2-necked RBF equipped with reflux condenser and inert atmosphere, 2,2-dimethyl-1,3-dioxane-4,6-dione (2.33 g, 16 mmol) was dissolved in triethyl orthoformate (16 ml, 97 mmol) and the mixture was stirred at 100° C. under nitrogen for 1.5 h. On complete consumption of starting material (tic), pyridin-4-amine (1.5 g, 16 mmol) was added and heating continued for 4.5 h. The reaction mixture was cooled down to RT and poured into hexane (50 mL). The solid was filtered off and washed with hexane to afford 2,2-dimethyl-5-((pyridin-4-ylamino)methylene)-1,3-dioxane-4,6-dione as an orange solid.

Aufarbeitung

  1. customIn a dried 2-necked RBF equipped
  2. temperaturewith reflux condenser
  3. additionwas added
  4. temperatureheating
  5. waitcontinued for 4.5 h
  6. temperatureThe reaction mixture was cooled down to RT
  7. filtrationThe solid was filtered off
  8. washwashed with hexane

Quellen und Nachweise

ORD-Eintrag
ord-108d9963829949a7a3e528f877daf3c9
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07981891B2

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