HRID566174

反应详情

EQUATION

反应方程式

HRID 566174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 200 mL microjar, 4.73 g of D,L-allysine ethylene acetal and 4.1 mg of catalase (derived from bovine liver, Sigma) were dissolved in 100 mL of 10 mM phosphate buffer (pH 8.3). Then, 2.37 g of immobilized D-amino acid oxidase (of the Trigonopsis origin, Boehringer Mannheim) was added and the reaction was conducted with stirring and 0.5 mL/min. aeration at 25° C. for 12 hours. This reaction mixture was filtered and the filtrate was subjected to HPLC analysis. The substrate residue rate was 50%. The filtrate was also concentrated under reduced pressure, added methanol, and stirred under cooling with ice bath, and the precipitated L-allysine ethylene acetal was collected by filtration and dried to provide 1.73 g of pure L-allysine ethylene acetal. By HPLC analysis, the chemical purity of this product was found to be 99% (Finepak SIL C18-5, Nippon Bunko), and the optical purity was 100% e.e. (CROWNPAK CR(+), Daicel).

WORKUP

后处理

  1. filtrationThis reaction mixture was filtered
  2. concentrationThe filtrate was also concentrated under reduced pressure
  3. additionadded methanol
  4. stirringstirred
  5. temperatureunder cooling with ice bath
  6. filtrationthe precipitated L-allysine ethylene acetal was collected by filtration
  7. customdried