| 摘要 |
PURPOSE:To obtain the titled compound easily in high yield, by reacting pyroglutamylhistidine hydrazide with an alkyl nitrite in the presence of hydrogen chloride, reacting a tertiary lower alkylamine and glycine with the reaction product, adding water thereto, and concentrating the resultant reaction mixture. CONSTITUTION:Pyroglutamylhistidine hydrazide of formula I as a raw material is reacted with an alkyl nitrite, e.g. amyl nitrite, in the presence of hydrogen chloride to give an azide of formula II, which is then reacted with a tertiary lower alkylamine, e.g. triethylamine (TEA), and glycine. Water is then added thereto, and the resulant reaction mixture is concentrated to afford the aimed compound of formula III. The reaction is carried out by dissolving the compound of formula I in dimethylformamide (DMF) or dimethyl sulfoxide (DMSO), adding a slight excess of an alkyl nitrite in a solution of tetrahydrofuran (THF) containing 2-4 equivalents HC1 at -20--50 deg.C to the solution to form an azide, adding the tertiary lower alkylamine and glycine thereto, and carrying out the coupling reaction at 0--50 deg.C.
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