HRID904944
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
4.35 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
- filtrationAfter filtering the mixture
- customthe solvent is removed by distillation
- washwashed successively with 2 N acetic acid, 1 M sodium bicarbonate and water
- dry with materialdried over sodium sulfate
- customafter removing the ethyl acetate
- distillationby distillation
- customis recrystallized from diisopropyl ether