HRID653548
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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°.
WORKUP
后处理
- temperaturemaintaining the pot temperature below 35° C
- temperaturethe slurry was cooled to 0°-5° C.
- waitheld for 0.5 hr
- customSolid β-methyl-L-aspartate hydrochloride was collected
- washwashed with 100 ml of isopropyl acetate
- customDry wt.=100.2 g (70.6%) m.p. 192°-4°