HRID1271656

反应详情

EQUATION

反应方程式

HRID 1271656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

L-Ala-OMe HCl salt (1.00 g, 7.16 mmol) was suspended in methyl acetate (15 ml). 4-Ethylbenzenesulfonic acid (4-EBS) (1.60 g, 8.57 mmol) was added, and the mixture was stirred for dissolution. This solution was concentrated under reduced pressure, methyl acetate (15 ml) was added, and the mixture was concentrated twice under reduced pressure. The obtained concentrate was cooled in a refrigerator. Since partial crystallization occurred, methyl acetate (15 ml) was added to dissolve the crystals at 50° C. This solution was stirred at room temperature to give a slurry. This slurry was cooled overnight in a refrigerator and the crystals were separated and dried to give 1.04 g of L-alanine methyl ester 4-ethylbenzenesulfonate (L-Ala-OMe 4-EBS salt) dry crystals (L-Ala-OMe 4-EBS salt content 100%, 3.42 mmol, yield 47.8%).

WORKUP

后处理

  1. concentrationThis solution was concentrated under reduced pressure, methyl acetate (15 ml)
  2. additionwas added
  3. concentrationthe mixture was concentrated twice under reduced pressure
  4. concentrationThe obtained concentrate
  5. temperaturewas cooled in a refrigerator
  6. customSince partial crystallization
  7. additionmethyl acetate (15 ml) was added
  8. dissolutionto dissolve the crystals at 50° C
  9. stirringThis solution was stirred at room temperature
  10. customto give a slurry
  11. temperatureThis slurry was cooled overnight in a refrigerator
  12. customthe crystals were separated
  13. customdried