HRID972703
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
4 ml of n-hexyl amine were added at 0° C. to a solution of 3.1 g of L-pyroglutamic acid 2,4,5-trichlorophenyl ester in 10 ml of dimethyl formamide and the solution was left at room temperature for 20 hours. The solvent was removed by distillation in vacuo at room temperature. The residue was taken up in 90% aqueous methanol, and the solution was filtered successively through 200 ml each of Levatit S 100(H+ -form)and Serdolit Blau (OH- -form). The ion exchanger columns were washed with 200 ml of 90% methanol and the combined eluate and washing solution were concentrated in vacuo. The L-pyroglutamic acid n-hexyl amide obtained as a colorless solid was recrystallized from ethyl acetate.
WORKUP
后处理
- customThe solvent was removed by distillation in vacuo at room temperature
- filtrationthe solution was filtered successively through 200 ml each of Levatit S 100(H+ -form)and Serdolit Blau (OH- -form)
- washThe ion exchanger columns were washed with 200 ml of 90% methanol
- washthe combined eluate and washing solution
- concentrationwere concentrated in vacuo