反应详情

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

1. stirringthe resulting mixture was stirred for a further two days
2. customAfter removal of the solvent in vacuo the crude product
3. customobtained
4. customwas purified by flash chromatography (silica gel; methylene chloride/ethanol=10:1 to 4:1)