HRID720161

反应详情

EQUATION

反应方程式

HRID 720161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of (S,S)-3-naphthalen-2-yl-2-[2-(2-nitro-benzenesulfonylamino)-pent-4-enoylamino]-propionic acid methyl ester, 3, (3.6 g, 7.0 mmol) and 1,2-dibromoethane (13.2 g, 70.0 mmol) in DMF (40 mL) is added potassium carbonate (9.6 g, 70.0 mmol). The reaction suspension was stirred at 65° C. for 12 h, quenched with 10% aqueous HCl and extracted with EtOAc. The extract is dried over Na2SO4, concentrated and the residue purified over silica gel (hexanes/EtOAc,1:2) to afford 3.7 g (97% yield) of the desired product.

WORKUP

后处理

  1. customquenched with 10% aqueous HCl
  2. extractionextracted with EtOAc
  3. dry with materialThe extract is dried over Na2SO4
  4. concentrationconcentrated
  5. customthe residue purified over silica gel (hexanes/EtOAc,1:2)