反应详情

温度

80 °C

165.19 g (1.00 mol) of 2-(3-aminophenyl)-1,3-dioxolan (CA 108 (15): 131815 r), 156.35 g (3.00 mol) of pulverized potassium hydroxide and 11.39 g (0.05 mol) of benzyltriethylammonium chloride are vigorously mechanically stirred under argon and heated to 80° C. 543.09 g (3.00 mol) of bromoacetic acid isopropyl ester is instilled in the suspension and the reaction mixture is stirred for about 8 hours at 80° C. Then, it is filtered, the filtrate is shaken out several times with concentrated aqueous sodium bicarbonate solution, the organic phase is dried on anhydrous magnesium sulfate, filtered and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel 60 (Merck) with methylene chloride/methanol. After concentration by evaporation, the product fractions yield a colorless oil.

1. filtrationThen, it is filtered
2. stirringthe filtrate is shaken out several times with concentrated aqueous sodium bicarbonate solution
3. dry with materialthe organic phase is dried on anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated by evaporation in a vacuum
6. customThe residue is chromatographed on silica gel 60 (Merck) with methylene chloride/methanol
7. concentrationAfter concentration
8. customby evaporation
9. customthe product fractions yield a colorless oil