反应详情

Next, 1.25 g (1.94 mmol) of benzyl 2-(N-benzyloxycarbonylamino)-4-{[4-(benzyloxycarbonylmethyl)phenyl] (methyl)phosphono}butanoate was dissolved in 20 mL of acetic acid and mixed with 200 mg of 5% palladium-carbon and hydrogen gas was introduced at room temperature for 3.5 hours. Thereafter, the palladium-carbon was removed by Celite filtration and the filtrate was vacuum-concentrated and the residue was purified by medium pressure reversed-phase chromatography (ODS-S-50B). The column was eluted with a linear gradient of 30 to 60% methanol at a flow rate of 6 mL/min and the fractions of the compound eluted with 60% methanol were collected. The elution and purity of the compound were confirmed by TLC (BuOH/AcOH/H2O=5:2:2, ninhydrin coloration). After vacuum concentration, freeze drying from water were carried out to obtain 2-amino-4-{[4-(carboxymethyl)phenyl](methyl)phosphono}butanoic acid (0.41 g, yield 64%) as a colorless solid.

1. additionwas introduced at room temperature for 3.5 hours
2. customThereafter, the palladium-carbon was removed by Celite filtration
3. concentrationthe filtrate was vacuum-concentrated
4. customthe residue was purified by medium pressure reversed-phase chromatography (ODS-S-50B)
5. washThe column was eluted with a linear gradient of 30 to 60% methanol at a flow rate of 6 mL/min
6. washthe fractions of the compound eluted with 60% methanol
7. customwere collected
8. washThe elution and purity of the compound
9. concentrationAfter vacuum concentration, freeze
10. dry with materialdrying from water