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Next, 0.57 g (1.05 mmol) of benzyl 2-(N-4-nitrobenzyloxycarbonylamino)-4-[methyl(phenyl)phosphono]butanoate was dissolved in 20 mL of acetic acid and mixed with 210 mg of 10% palladium-carbon and hydrogen gas was introduced for 2 hours. The palladium-carbon was removed by Celite filtration and the filtrate was concentrated in reduced pressure. The residue was purified by medium pressure reversed-phase column chromatography ODS-S-50B. The column was eluted with a linear gradient of 4 to 50% acetonitrile (12 mL/min flow rate) and the fractions of the compound eluted with 5% acetonitrile were collected and the elution and purity of the compound were confirmed by TLC (BuOH/AcOH/H2O=5:2:2, ninhydrin coloration). After vacuum concentration, freeze drying was carried out to obtain 2-amino-4-[methyl(phenyl)phosphono]butanoic acid (0.14 g, yield 48%) as a colorless solid.

1. additionwas introduced for 2 hours
2. customThe palladium-carbon was removed by Celite filtration
3. concentrationthe filtrate was concentrated in reduced pressure
4. customThe residue was purified by medium pressure reversed-phase column chromatography ODS-S-50B
5. washThe column was eluted with a linear gradient of 4 to 50% acetonitrile (12 mL/min flow rate)
6. washthe fractions of the compound eluted with 5% acetonitrile
7. customwere collected
8. washthe elution and purity of the compound
9. concentrationAfter vacuum concentration, freeze
10. customdrying