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
1.75 g of DCC are added to a solution of 2.14 g of Z-(L)-Val-OH in 80 ml of absolute ice-cooled methylene chloride and after stirring for 20 minutes at that temperature a solution of 2 g of H-(L)-Phe-morpholin-4-ylamide is added dropwise thereto over a period of 15 minutes. The reaction mixture is stirred for a further 24 hours at room temperature and the urea that forms is filtered off. The filtrate is washed in succession with aqueous sodium hydrogen carbonate solution and brine and, after drying over sodium sulfate, concentrated. Stirring with ether and removal of the insoluble residue by filtration yields, after concentration, the title compound which is processed further without additional purification. TLC Rf (D )=0.7.
WORKUP
后处理
- additionis added dropwise
- filtrationthe urea that forms is filtered off
- washThe filtrate is washed in succession with aqueous sodium hydrogen carbonate solution and brine
- dry with materialafter drying over sodium sulfate
- concentrationconcentrated
- stirringStirring with ether and removal of the insoluble residue by filtration
- customyields
- concentrationafter concentration
- customthe title compound which is processed further without additional purification