Sodium Hydroxide → HCID 2762294, compound

In 10 ml of methanol was dissolved 0.5 g of isopropyl (2S, 3S)-3-(N-Boc)amino-4-phenyl-2-hydroxybutyrate, followed by addition of 1.38 g of aqueous 3N sodium hydroxide solution, and the resulting mixture was washed at room temperature for 2 hours for the promotion of the hydrolysis reaction. After the termination of the reaction was confirmed, aqueous 1N hydrochloric acid solution was added to the resulting mixture to adjust the mixture to pH 3.0, followed by concentration under reduced pressure. The concentrate was diluted with ethyl acetate and water, followed by layer separation, and the resulting ethyl acetate layer was washed with saturated sodium chloride solution. Furthermore, the ethyl acetate layer was dried over anhydrous magnesium sulfate, filtered and concentrated, to obtain (2S, 3S)-3-(N-Boc)amino-4-phenyl-2-hydroxybutyric acid of 0.38 g in a yield of 86.9%. The NMR analysis is shown below.

1. washthe resulting mixture was washed at room temperature for 2 hours for the promotion of the hydrolysis reaction
2. additionaqueous 1N hydrochloric acid solution was added to the resulting mixture
3. concentrationfollowed by concentration under reduced pressure
4. additionThe concentrate was diluted with ethyl acetate and water
5. customfollowed by layer separation
6. washthe resulting ethyl acetate layer was washed with saturated sodium chloride solution
7. dry with materialFurthermore, the ethyl acetate layer was dried over anhydrous magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated

ORD record

ord-2605a33d9c6a48c988bbbd916532150c

Source dataset

uspto-grants-2000_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06063955