Diethyl (3-chloropropyl)phosphonate

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of diethyl 3-chloropropylphosphonate (430.6 g) in dry N,N-dimethyformamide (2.25 l) was added potassium salt of ethyl N-ethoxycarbonyloxycarbamate (429.2 g). This mixture was stirred at 64°-66° C. for three hours. After the resulting potassium chloride was removed by filtration, the filtrate was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (2.0 l) and washed with water (4.0 l). The aqueous layer was extracted twice with ethyl acetate (1.2 and 0.8 l). The combined ethyl acetate layer was washed with saturated aqueous sodium chloride solution (1.5 l), dried over magnesium sulfate and concentrated under reduced pressure to give oily diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)propylphosphonate (643.7 g). After the resulting potassium chloride was removed by filtration the filtrate was concentrated under reduced pressure The residue was dissolved in ethyl acetate (2.0 l) washed with water (4.0 l) The aqueous layer was extracted twice with ethyl acetate (1.2 and 0.8 l) The combined ethyl acetate layer was washed with saturated aqueous sodium chloride solution (1.5 l) dried over magnesium sulfate concentrated under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of diethyl 3-chloropropylphosphonate (430.6 g) in dry N,N-dimethylformamide (2.25 l) was added potassium salt of ethyl N-ethoxycarbonyloxycarbamate (429.2 g). This mixture was stirred at 64°-66° C. for three hours. After the resulting potassium chloride was removed by filtration, the filtrate was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (2.0 l) and washed with water (4.0 l). The aqueous layer was extracted twice with ethyl acetate (1.2 and 0.8 l). The combined ethyl acetate layer was washed with saturated aqueous sodium chloride solution (1.5 l), dried over magnesium sulfate and concentrated under reduced pressure to give oily diethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-propylphosphonate (643.7 g). After the resulting potassium chloride was removed by filtration the filtrate was concentrated under reduced pressure The residue was dissolved in ethyl acetate (2.0 l) washed with water (4.0 l) The aqueous layer was extracted twice with ethyl acetate (1.2 and 0.8 l) The combined ethyl acetate layer was washed with saturated aqueous sodium chloride solution (1.5 l) dried over magnesium sulfate concentrated under reduced pressure