HRID1585320

反应详情

EQUATION

反应方程式

HRID 1585320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3.00 g (7.05 mmol) of 5(S)-[1(S)-(Boc-amino)-2-(p-methoxy-phenyl)-ethyl]-3(R)-(phenylmethyl)dihydrofuran-2-(3H)-one in 112 ml of dimethoxyethane and 57 ml of water are hydrolysed, under protective gas, with 28 ml of 1 M lithium hydroxide solution. After 20 h at RT, the reaction mixture is poured onto an ice-cold mixture of 340 ml of sat. NH4Cl solution, 28 ml of 10% citric acid solution and 140 ml of methylene chloride. Methanol is added in order to dissolve the product completely. The aqueous phase is separated off and extracted 2× with methylene chloride. The organic phases are washed with saline, dried with Na2SO4 and evaporated, with the title compound being obtained: tRet (II)=14.0 min; FAB-MS (M+H)+ =444.

WORKUP

后处理

  1. dissolutionto dissolve the product completely
  2. customThe aqueous phase is separated off
  3. extractionextracted 2× with methylene chloride
  4. washThe organic phases are washed with saline
  5. dry with materialdried with Na2SO4
  6. customevaporated, with the title compound
  7. custombeing obtained