反应详情

1.41 g of 3,5-dichlorobenzaldehyde are added to a solution of 2.53 g of 3-aminopropyl(diethoxymethyl)-phosphinic acid ethyl ester in 10 ml of anhydrous methanol and the resulting clear solution is stirred at room temperature for 30 minutes. There are then added first 0.6 g of glacial acetic acid and then, dropwise, 0.21 g of sodium cyanoborohydride dissolved in 5 ml of methanol. An exothermic reaction begins. The reaction mixture is stirred for 3 hours at 20°, adjusted to pH 8, and the solvent is removed. The residue is dissolved in dichloromethane and washed with water. The organic phase is separated off, dried over sodium sulfate and concentrated to dryness by evaporation. The oil that remains behind is purified by chromatography on silica gel, yielding 3-(3,5-dichlorobenzylamino)propyl(diethoxymethyl)-phosphinic acid ethyl ester in the form of a yellowish oil.

1. customAn exothermic reaction
2. stirringThe reaction mixture is stirred for 3 hours at 20°
3. customthe solvent is removed
4. dissolutionThe residue is dissolved in dichloromethane
5. washwashed with water
6. customThe organic phase is separated off
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated to dryness by evaporation
9. customThe oil that remains behind is purified by chromatography on silica gel