HRID904944

反应详情

EQUATION

反应方程式

HRID 904944 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.35 g of Boc-Val-OH and 6.6 g of H-Lys(Z)-OMe.HCl are subjected to a condensation reaction with 4.4 g of DCC in 50 ml of CH2Cl2, with the addition of 2.7 g of HOBt and 2.6 ml of N-ethylmorpholine (NEM). After filtering the mixture, the solvent is removed by distillation. The residue is taken up in ethyl acetate, washed successively with 2 N acetic acid, 1 M sodium bicarbonate and water and dried over sodium sulfate and, after removing the ethyl acetate by distillation, is recrystallized from diisopropyl ether. Yield 3.5 g, melting point 100°-102°, elementary analysis (C, H and N) correct.

WORKUP

后处理

  1. filtrationAfter filtering the mixture
  2. customthe solvent is removed by distillation
  3. washwashed successively with 2 N acetic acid, 1 M sodium bicarbonate and water
  4. dry with materialdried over sodium sulfate
  5. customafter removing the ethyl acetate
  6. distillationby distillation
  7. customis recrystallized from diisopropyl ether