HRID2280355

反应详情

EQUATION

反应方程式

HRID 2280355 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Into a 250 mL round-bottomed flask equipped with a stirrer, reflux condenser and thermometer was added O-methyl-D,L-serine (5 g) in 90:10 methanol/water (25 mL). N-Acetyl-D-phenylalanine (8.70 g) was added in one portion and the mixture heated to 50° C. overnight. The suspension was cooled to room temperature and filtered, and the solid was rinsed with 90:10 methanol/water (5 mL) and dried at 40° C. under vacuum for 3 h. The N-acetyl-D-phenylalanine salt of O-methyl-D-serine (3.4 g, 25%) was obtained as a white solid with a chiral purity >90%. Regeneration of the title compound could be effected by adjustment of the pH to 1-2 by treatment with HCl, followed by extraction into an organic solvent and subsequent adjustment of the pH to ˜7 with NaOH.

WORKUP

后处理

  1. customInto a 250 mL round-bottomed flask equipped with a stirrer
  2. temperaturereflux condenser
  3. temperatureThe suspension was cooled to room temperature
  4. filtrationfiltered
  5. washthe solid was rinsed with 90:10 methanol/water (5 mL)
  6. customdried at 40° C. under vacuum for 3 h