HRID1528

反应详情

EQUATION

反应方程式

HRID 1528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-(2-t-Butoxycarbonylaminoethyl)phenoxymethylphosphonic acid, diethyl ester (2.856 g, 9.95 mMol) in methylene chloride (300 ml) and trifluoracetic acid (16 ml) was stirred at room temperature for 5 h. The solution was concentrated under reduced pressure and product dried under in vacuo. The trifluoacetic acid salt was neutralized with aqueous sodium carbonate and extracted with dichloromethane containing a small proportion of methanol (5×100 ml). The combined organic layers were dried over sodium sulfate and evaporated to dryness to give the title compound as a pale yellow gum.

WORKUP

后处理

  1. concentrationThe solution was concentrated under reduced pressure and product
  2. customdried under in vacuo
  3. extractionextracted with dichloromethane containing a small proportion of methanol (5×100 ml)
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. customevaporated to dryness