HRID977519

反应详情

EQUATION

反应方程式

HRID 977519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of H-DNle-OBzl.TsOH (1.27 g) in dichloromethane (20 ml) were added NMM (0.53 ml), Boc-DTrp-OH (1.22 g), HOBT.H2O (734 mg) and EDCI.HCl (926 mg) successively under ice cooling. The mixture was stirred at the same temperature for 1 h and at room temperature for 2 h. The mixture was diluted with ethyl acetate, washed with sat. aq. NaHCO3, 10% aq. citric acid, and brine successively, dried over MgSO4 and evaporated in vacuo. The residue was recrystallized from ethyl acetate and hexane to give Boc-DTrp-DNle-OBzl (1.56 g).

WORKUP

后处理

  1. washwashed with sat. aq. NaHCO3, 10% aq. citric acid, and brine successively
  2. dry with materialdried over MgSO4
  3. customevaporated in vacuo
  4. customThe residue was recrystallized from ethyl acetate and hexane