HRID502306

反应详情

EQUATION

反应方程式

HRID 502306 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N—(N-Acetyl-tyrosinyl-valinyl-(4-benzyloxyprolinyl))-3-amino-4-oxobutanoic acid tert-butyl ester semicarbazone (270 mg) was dissolved into 10 ml of 25% trifluoroacetic acid in dichloromethane and stirred at room temperature for 3 hours. The mixture was concentrated to give a solid residue. The residue was dissolved into a 10 ml mixture of methanol:acetic acid: 37% formaldehyde (3:1:1) and stirred at room temperature for 1 hour. The mixture was concentrated and the resulting residue purified by flash chromatography (SiO2) eluting with dichloromethane/methanol/formic acid (100:5:0.5) to give 37 mg of the title compound.

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. customto give a solid residue
  3. concentrationThe mixture was concentrated
  4. customthe resulting residue purified by flash chromatography (SiO2)
  5. washeluting with dichloromethane/methanol/formic acid (100:5:0.5)