(3-氨丙基)磷酸二乙酯

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:

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: A mixture of diethyl[3-(N-phthalimido)]propylphosphonate (ex. 5) (3.72 g; 11.4 mmoles), absolute ethanol (46 ml) and hydrazine hydrate (0.78 ml of 98% purity; 15.7 mmoles) is stirred at reflux for 35 min. The mixture is filtered and the solvent is distilled under vacuo. The resulting oil is dissolved in CHCl3 (10 ml) and is filtered again. Solvent removal in vacuo gives a colorless liquid (0.7 g; yield 30%). According to example 4, diethyl 3-aminopropylphosphonate (6) is also obtained from diethyl 2-cyanoethylphosphonate in an analogous fashion followed by vacuum distillation at about 115° C. and 0.18 mbar (yield 80%). at reflux for 35 min The mixture is filtered the solvent is distilled under vacuo The resulting oil is dissolved in CHCl3 (10 ml) is filtered again Solvent removal in vacuo gives a colorless liquid (0.7 g; yield 30%)

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: 97 g. of 3-aminopropanephosphonic acid diethyl ester is dissolved in 400 ml. of dry pyridine and 55 g. of acetic anhydride is added with stirring. The mixture is then boiled for 4 hours with refluxing and freed of the low-boiling components by evaporation in a light vacuum. Gaschromatographically pure N-acetyl-3-aminopropanephosphonic acid diethyl ester is obtained in a 96% yield by shortcut distillation in vacuo. It is a pale yellow, highly viscous oil with a boiling point of 166° to 160° C. (0.4 Torr). with refluxing freed of the low-boiling components by evaporation in a light vacuum

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

实验步骤: A mixture of diethyl[3-(N-phthalimido)]propylphosphonate (ex. 5) (3.72 g; 11.4 mmoles), absolute ethanol (46 ml) and hydrazine hydrate (0.78 ml of 98% purity; 15.7 mmoles) is stirred at reflux for 35 min. The mixture is filtered and the solvent is distilled under vacuo. The resulting oil is dissolved in CHCl3 (10 ml) and is filtered again. Solvent removal in vacuo gives a colorless liquid (0.7 g; yield 30%). According to example 4, diethyl 3-aminopropylphosphonate (6) is also obtained from diethyl 2-cyanoethylphosphonate in an analogous fashion followed by vacuum distillation at about 115° C. and 0.18 mbar (yield 80%). at reflux for 35 min The mixture is filtered the solvent is distilled under vacuo The resulting oil is dissolved in CHCl3 (10 ml) is filtered again Solvent removal in vacuo gives a colorless liquid (0.7 g; yield 30%)

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

实验步骤: A mixture of diethyl[3-(N-phthalimido)]propylphosphonate (ex. 5) (3.72 g; 11.4 mmoles), absolute ethanol (46 ml) and hydrazine hydrate (0.78 ml of 98% purity; 15.7 mmoles) is stirred at reflux for 35 min. The mixture is filtered and the solvent is distilled under vacuo. The resulting oil is dissolved in CHCl3 (10 ml) and is filtered again. Solvent removal in vacuo gives a colorless liquid (0.7 g; yield 30%). According to example 4, diethyl 3-aminopropylphosphonate (6) is also obtained from diethyl 2-cyanoethylphosphonate in an analogous fashion followed by vacuum distillation at about 115° C. and 0.18 mbar (yield 80%). at reflux for 35 min The mixture is filtered the solvent is distilled under vacuo The resulting oil is dissolved in CHCl3 (10 ml) is filtered again Solvent removal in vacuo gives a colorless liquid (0.7 g; yield 30%)

反应条件: temp:117.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Following General Procedure D, Compound 47 (50 mg, 0.12 mmol) and diethyl 3-aminopropylphosphonate (69 mg, 0.36 mmol) in n-BuOH (3 mL) were heated to 117° C. for 24 h with a reflux condenser. The product (Compound 81) was purified by preparative silica gel TLC plate 1000μ using 5% (7N NH3-MeOH) and 95% CH2Cl2 solution as eluent. The product (Compound 81) was purified by preparative silica gel TLC plate

反应条件: temp:117.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Following General Procedure D, Compound 47 (50 mg, 0.12 mmol) and diethyl 3-aminopropylphosphonate (69 mg, 0.36 mmol) in n-BuOH (3 mL) were heated to 117° C. for 24 h with a reflux condenser. The product (Compound 81) was purified by preparative silica gel TLC plate 1000μ using 5% (7N NH3-MeOH) and 95% CH2Cl2 solution as eluent. The product (Compound 81) was purified by preparative silica gel TLC plate