반응 #480845

반응 방정식

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

수율 96.4%

용매

isopropanol

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도at reflux for 30 minutes
3. 3
   workup.WAITThe mixture was left
4. 4
   온도to cool to ambient temperature overnight
5. 5
   기타The precipitate formed
6. 6
   여과was collected by filtration
7. 7
   세척washed with isopropanol
8. 8
   기타dried under vacuum

실험 절차

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%).

출처