反应详情

To a stirred solution of 2.25 g (9.3 mmol) of 1-(benzyloxycarbonylamino)ethylphosphonous acid in 70 ml of methylene chloride, were added triethylamine (2.87 ml, 20 mmol), trimethylsilyl chloride (2.60 ml, 20 mmol), and methyl 2-bromomethylacrylate (1.66 g, 9.3 mmol) at 0° C. After stirring at room temperature for 20 hours, the reaction mixture was washed with H2O, 2N HCl, and then saturated NaCl solution and dried over anhydrous magnesium sulfate. The mixture obtained by filtration and evaporation was purified by silica gel chromatography (eluted with chloroform followed by 10% methanol-chloroform) to give 2.50 g (yield 79%) of the product.

1. washthe reaction mixture was washed with H2O, 2N HCl
2. dry with materialsaturated NaCl solution and dried over anhydrous magnesium sulfate
3. customThe mixture obtained by filtration and evaporation
4. customwas purified by silica gel chromatography (eluted with chloroform followed by 10% methanol-chloroform)