反应详情

To this end, 23.08 g (46.1 mmol) of hydrazine monohydrate are added dropwise to 15 g (46.1 mmol) of diethyl phthalimidopropylphosphonate in about 500 ml of absolute ethanol. The reaction medium is stirred for 12 hours. The salts formed are filtered off and washed with ethanol. After evaporating off the ethanol, salts are again formed. These salts are washed with CH2Cl2 and filtered on a Millipore membrane (0.45 μm). The filtrate is recovered and the CH2Cl2 is evaporated off. A yellow oil is obtained. The crude product is purified by chromatography on a column of silica gel with a 90/10 CHCl3/MeOH mixture as eluent. 4.6 g of diethyl 3-aminopropylphosphonate (APPE) are obtained in a yield of 51.8%.

1. customThe salts formed
2. filtrationare filtered off
3. washwashed with ethanol
4. customAfter evaporating off the ethanol, salts
5. customare again formed
6. washThese salts are washed with CH2Cl2
7. filtrationfiltered on a Millipore membrane (0.45 μm)
8. customThe filtrate is recovered
9. customthe CH2Cl2 is evaporated off
10. customA yellow oil is obtained
11. customThe crude product is purified by chromatography on a column of silica gel with a 90/10 CHCl3/MeOH mixture as eluent