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
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
- filtrationThis reaction mixture was filtered
- concentrationThe filtrate was also concentrated under reduced pressure
- additionadded methanol
- stirringstirred
- temperatureunder cooling with ice bath
- filtrationthe precipitated L-allysine ethylene acetal was collected by filtration
- customdried