HRID1066042

反应详情

EQUATION

反应方程式

HRID 1066042 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (3S)-3-[N-((1-naphthylamino)acetyl)leucinyl]amino-4-oxobutanoic acid tert-butyl ester semicarbazone (0.201 g, 0.38 mmol) in CH2Cl2(2.0 mL)-anisole(0.5 mL) at room temperature under nitrogen was added trifluoroacetic acid (2.0 mL). The resulting solution was stirred at room temperature for 5 hrs, evaporated to dryness and chased with CH2Cl2 and toluene-CH2Cl2 (1:1). The resulting solid was triturated with CH2Cl2—Et2O to give the title compound (0.176 g, 98%) as a pale gray solid. TLC(EtOAc-pyridine-AcOH—H2O; 60:20:5:10) Rf=0.45.

WORKUP

后处理

  1. customevaporated to dryness and chased with CH2Cl2 and toluene-CH2Cl2 (1:1)
  2. customThe resulting solid was triturated with CH2Cl2—Et2O