HRID50331

反应详情

EQUATION

反应方程式

HRID 50331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.15 g (0.27 mmol) of 2-[(4-amidinophenyl)thiomethyl]benzothiazol-5-yl-carboxylic acid-N-phenyl-N-(2-ethoxycarbonylethyl)amide hydrochloride in 10 mL of acetic acid was mixed with 0.09 mL (about 0.81 mmol) of 30% hydrogen peroxide solution and stirred at room temperature. After 4 days, a further 0.18 mL of hydrogen peroxide solution was added and the resulting mixture was stirred for a further two days. After removal of the solvent in vacuo, the crude product obtained was purified by flash chromatography (silica gel; methylene chloride/ethanol=10:1 to 4:1). Yield: 58% of theory, C27H26N4O4S2 (534.66); Rf value: 0.24 (silica gel; methylene chloride/ethanol=4:1+a few drops of acetic acid); EKA mass spectrum: (M+H)+=535.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred for a further two days
  2. customAfter removal of the solvent in vacuo