反应详情

温度

60 °C

A solution of 5-((3-hydroxy-4-methoxyanilino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione, (prepared as described for the starting material in Example 3), 4-(3-chloropropyl)morpholine hydrochloride (680 mg, 3.57 mmol), (J. Amer. Chem. Soc. 1945, 67, 736), in DMF (25 ml) containing potassium carbonate (940 mg, 7.48 mmol) and potassium iodide (56 mg, 0.34 mmol) was stirred at 60° C. for 2 hours. The mixture was partitioned between ethyl acetate and water. The organic layer was separated, washed with brine, dried (MgSO4), the insoluble materials were removed by filtration and the volatiles were removed by evaporation. The residue was triturated with ether, collected by filtration and dried under vacuum to give 5-((3-(3-morpholinopropoxy)-4-methoxyanilino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione 2735 mg, 5 1%).

1. customThe mixture was partitioned between ethyl acetate and water
2. customThe organic layer was separated
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. customthe insoluble materials were removed by filtration
6. customthe volatiles were removed by evaporation
7. customThe residue was triturated with ether
8. filtrationcollected by filtration
9. customdried under vacuum