HRID972703

反应详情

EQUATION

反应方程式

HRID 972703 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed by distillation in vacuo at room temperature
  2. filtrationthe solution was filtered successively through 200 ml each of Levatit S 100(H+ -form)and Serdolit Blau (OH- -form)
  3. washThe ion exchanger columns were washed with 200 ml of 90% methanol
  4. washthe combined eluate and washing solution
  5. concentrationwere concentrated in vacuo