HRID653548

反应详情

EQUATION

反应方程式

HRID 653548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  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°