Reaktion #480845

Reaktionsgleichung

3-Methoxy-4-methoxycarbonylaniline

2,2-Dimethyl-5-methoxymethylene-1,3-dioxane-4,6-dione

→

5-((3-methoxy-4-methoxycarbonylanilino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione

Ausbeute 96.4%

Lösungsmittel

isopropanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture was heated
2. 2
   Temperaturat reflux for 30 minutes
3. 3
   workup.WAITThe mixture was left
4. 4
   Temperaturto cool to ambient temperature overnight
5. 5
   SonstigeThe precipitate formed
6. 6
   Filtrationwas collected by filtration
7. 7
   Waschenwashed with isopropanol
8. 8
   Sonstigedried under vacuum

Vorschrift

3-Methoxy-4-methoxycarbonylaniline (14.15 g, 78 mmol) was suspended in isopropanol and heated at 50° C. 2,2-Dimethyl-5-methoxymethylene-1,3-dioxane-4,6-dione (14.8 g, 80 mmol), (Montatsh. Chem. 1967, 98, 564), was then added in portions over 10 minutes and the mixture was heated at reflux for 30 minutes. The mixture was left to cool to ambient temperature overnight. The precipitate formed was collected by filtration, washed with isopropanol and dried under vacuum to give 5-((3-methoxy-4-methoxycarbonylanilino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (25.2 g, 96%).

Quelle