HRID1648379
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
To a stirring solution of EtOCO-D,L-Phe(αMe)-Pro-OBzl (13.2 g, 30 mmol) in p-dioxane (250 mL) was added a solution of LiOH.H2O (6.3 g, 151 mmol) in water (125 mL). After stirring for 2.5 h, the solvent was removed in vacuo and the residue was diluted with water and washed three times with diethyl ether. The aqueous phase was then taken to pH 2 with conc. HCl and extracted three times with ethyl acetate. The combined ethyl acetate extracts were dried (Na2SO4), filtered and concentrated in vacuo to give 10.7 g of a white solid.
WORKUP
后处理
- customthe solvent was removed in vacuo
- additionthe residue was diluted with water
- washwashed three times with diethyl ether
- extractionextracted three times with ethyl acetate
- dry with materialThe combined ethyl acetate extracts were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo