HRID1954679
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 solution of Cbz-D-hPro-N(Me)Gly-OEt (6 g, 16.6 mmol) in p-dioxane (200 mL) was added a solution of LiOH.H2O (2.78 g, 66.2 mmol) in water (100 mL) with vigorous stirring. After stirring for 12 hours, the solution was concentrated to a volume of 50 mL, diluted with water (100 mL), and extracted twice with diethyl ether (200 mL). The aqueous phase was adjusted to pH 2 with 5N aqueous HCl and extracted three times with ethyl acetate (150 mL). The combined ethyl acetate extracts were dried with MgSO4, filtered, and concentrated to give a white solid (5 g, 91%).
WORKUP
后处理
- concentrationthe solution was concentrated to a volume of 50 mL
- additiondiluted with water (100 mL)
- extractionextracted twice with diethyl ether (200 mL)
- extractionextracted three times with ethyl acetate (150 mL)
- dry with materialThe combined ethyl acetate extracts were dried with MgSO4
- filtrationfiltered
- concentrationconcentrated