反应详情

温度

80 °C

A mixture of 5-((3-hydroxy-4-methoxyanilino)methylene)-2,2-dimethyl-1,3dioxane-4,6-dione (10 g, 34.1 mmol), (prepared as described for the starting material in Example 3), 3-(pyrrolidin-1-yl)propyl chloride (7.55 g, 51.1 mmol), (J. Am. Chem. Soc. 1955, 77, 2272), potassium carbonate (7.06 g, 51.1 mmol) and potassium iodide (600 mg, 3.41 mmol) in DMF (100 ml) was heated at 80° C. for 2 hours. The mixture was poured into water (800 ml) and the precipitate was collected by filtration. The solid was dissolved in methylene chloride and the organic solution was washed with brine, dried (MgSO4) and the volatiles were removed by evaporation. The residue was dissolved in ether and the insoluble materials were removed by filtration. The volatiles were removed by evaporation and the residue was precipitated by trituration with petroleum ether, collected by filtration and dried under vacuum to give 5-((3-(3-pyrrolidin-1-ylpropoxy)-4-methoxyanilino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5.1 g, 37%).

1. custom(prepared
2. filtrationthe precipitate was collected by filtration
3. dissolutionThe solid was dissolved in methylene chloride
4. washthe organic solution was washed with brine
5. dry with materialdried (MgSO4)
6. customthe volatiles were removed by evaporation
7. dissolutionThe residue was dissolved in ether
8. customthe insoluble materials were removed by filtration
9. customThe volatiles were removed by evaporation
10. customthe residue was precipitated by trituration with petroleum ether
11. filtrationcollected by filtration
12. customdried under vacuum