Benzyl chloroformate → 3-(((Benzyloxy)carbonyl)amino)-2-methylpropanoic acid

Temperatur

0 °C

In a mixture of 10 ml of pyridine and 10 ml of water was dissolved 500 mg of β-amino-isobutyric acid, and 1.5 ml of benzyloxycarbonyl chloride was dropped thereinto with stirring at 0° C. After completion of the dropping, the resulting mixture was stirring of room temperature for 3 hours, after which the pyridine was removed under reduced pressure. Then, hydrochloric acid was added to the residue, and the resulting mixture was extracted with ethyl acetate. The ethyl acetate layer obtained was washed successively with diluted hydrochloric acid, water and an aqueous sodium chloride solution, and then concentrated to obtain an oily substance. Subsequently, the oily substance was washed with a mixed solvent of ether and hexane to obtain 380 mg of the desired compound.

1. additionwas dropped
2. stirringAfter completion of the dropping, the resulting mixture was stirring of room temperature for 3 hours
3. customafter which the pyridine was removed under reduced pressure
4. additionThen, hydrochloric acid was added to the residue
5. extractionthe resulting mixture was extracted with ethyl acetate
6. customThe ethyl acetate layer obtained
7. washwas washed successively with diluted hydrochloric acid, water
8. concentrationan aqueous sodium chloride solution, and then concentrated
9. customto obtain an oily substance
10. washSubsequently, the oily substance was washed with a mixed solvent of ether and hexane

ORD-Eintrag

ord-14531f34701b4a69bc63b6f70e00a2a5

Quelldatensatz

uspto-grants-1991_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05064945