HRID1418834

反应详情

EQUATION

反应方程式

HRID 1418834 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationthe solution was concentrated to a volume of 50 mL
  2. additiondiluted with water (100 mL)
  3. extractionextracted twice with diethyl ether (200 mL)
  4. extractionextracted three times with ethyl acetate (150 mL)
  5. dry with materialThe combined ethyl acetate extracts were dried with MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated