Zhu Hesun
2004
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Journal
Fine chemicals
Abstract
2-Aminobenzoic acid was firstly iodinated with KI and NaNO_2 in HCl to get 2-iodobenzoic acid in 92% yield,which was then oxidized by 2KHSO_5-KHSO_4-K_2SO_4 in aqueous solution at 70~73 ℃ to get 1-hydroxy-1,2-benziodoxol-3(1H)-one-1-oxide (IBX) in 81% yield.IBX was used at room tempereture as oxidant to oxidize 6α-bromopenicillanic acid to benzhydryl 6α-bromopenicillanate-1-oxide(Ⅰ).Benzhydryl penicillanate-1-oxide was eventually prepared by the treatment of Ⅰ with zinc dust under ultrasonic.In the synthetic process of Ⅰ,no separation of intermediate was made and the total yield was 82%.By using IBX as oxidant instead of peracetic acid,the reaction was carried out at room temperature instead of 0 ℃.The whole process is a green procedure and the molecular economics is improved.The product was corroborated by ~1HNMR and IR.