In my tlc with solvent system toluene:acetic acid:methanol(3:1:0.1 ratio) i m getting 2 spots for captopril sample...can anybody suggest good method of recystallisation to remove that "xtra spot"(impurity)
also if anybody can get me following full article access:
J Pharm Sci. 1984 Dec;73(12):1843-4.
An improved synthesis of captopril.
Nam DH, Lee CS, Ryu DD.
Abstract
An improved synthesis of captopril using methacrylic acid as the starting material is described. Treatment of methacrylic acid (I) with a hydrogen halide gave the 3-halogeno-2-methylpropanoic acids II and III, which were treated with thionyl chloride to yield the corresponding 3-halogeno-2-methylpropanoyl chlorides IV and V. Treatment of IV or V with L-proline yielded the N-(R,S-3-halogeno-2-methylpropanoyl)-L-prolines VI and VII, which were separated into optically pure R- and S-diastereoisomers using dicyclohexylamine. Treatment of halides of VI or VII with methanolic ammonium hydrosulfide gave captopril in 28% yield.