Hydrazine hydrate (1:1) → Diethyl (3-aminopropyl)phosphonate

참여 물질

반응 단계

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%.

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