Hydrochloric Acid → b-Methylaspartic acid hydrochloride

To methanol (500 ml) at 25°, gaseous HCl (0.89 mole) was bubbled into the solution over about 0.5 hr. L-Aspartic acid (0.77 mole) was added rapidly, then the resulting solution was held at 25° C. for 6.5 hrs. The methanol was stripped with an aspirator maintaining the pot temperature below 35° C. The batch became fairly thick when 145 ml (115 g) of methanol remained. Isopropyl acetate (435 ml) was added in about 0.5 hr, then the slurry was cooled to 0°-5° C. and held for 0.5 hr. Solid β-methyl-L-aspartate hydrochloride was collected and washed with 100 ml of isopropyl acetate. Dry wt.=100.2 g (70.6%) m.p. 192°-4°.

1. temperaturemaintaining the pot temperature below 35° C
2. temperaturethe slurry was cooled to 0°-5° C.
3. waitheld for 0.5 hr
4. customSolid β-methyl-L-aspartate hydrochloride was collected
5. washwashed with 100 ml of isopropyl acetate
6. customDry wt.=100.2 g (70.6%) m.p. 192°-4°

ORD record

ord-80a3fc6d8cb0443c956c5fee702e9079

Source dataset

uspto-grants-1987_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04677220