| 第 45 卷第 1 期 |  | Vol. 45 No. 1 | | 2015 年 2 月 | Feb 2015 |
|
所屬欄目：醫藥及中間體
頭孢他啶側鏈活性酯中一個(gè)未知雜質(zhì)的合成和確認 |
| 厲 昆1，李嘯風(fēng)2，任紅陽(yáng)1，江海波1
（1. 浙江普洛得邦制藥有限公司，浙江 東陽(yáng) 322118；2. 浙江大學(xué) 化學(xué)系，浙江 杭州 310027） |
| 摘 要：對合成頭孢他啶產(chǎn)生的雜質(zhì)頭孢他啶甲酯進(jìn)行了測定和推測，并對原料他啶側鏈活性酯（TAEM）進(jìn)行了追蹤分析，發(fā)現TAEM中有個(gè)未知雜質(zhì)，經(jīng)LC-MS和HPLC測定，證實(shí)這個(gè)雜質(zhì)的產(chǎn)生跟TAEM與甲醇溶媒有關(guān)系。據此合成了一個(gè)化合物，其結構經(jīng)LC-MS和HPLC確證。 |
| 關(guān)鍵詞：頭孢他啶；他啶側鏈活性酯；頭孢他啶甲酯 |
| 中圖分類(lèi)號：R978.1 文獻標識碼：A 文章編號：1009-9212（2015）01-0057-04 |
|
| Synthesis and Confirmation of an Unknown Impurity in(Z)-2-S-Benzothiazoly-2-(2-aminothiazol-4-yl)-2-(1-methoxy-2-methyl-1-oxopropan-2-yloxyimino)acetic Acid Ester |
| LI Kun1, LI Xiao-feng2, REN Hong-yang1, JIANG Hai-bo1
(1. Zhejiang Apeloa Tospo Pharm Co., Ltd., Dongyang 322118, China; 2. Department of Chemistry; Zhejiang University, Hangzhou 310027, China) |
| Abstract：The impurity(ceftazidime methyl)produced in the synthesis of ceftazidime were analyzed and speculated, and 2-Mercaptobenzothiazolyl-(Z)-(2-aminothiazol-4-yl)-2-(tert-butoxycarbonyl)isopropoxyiminoacetate(TAEM), a raw material for the synthesis of ceftazidime, was analyzed. The analytical results indicated that an unknown impurity existed in TAEM, and the experimental results from LC-MS and HPLC determination indicated that the existence of the impurity was related to a reaction between TAEM and methanol solvent. Based on the above deduction, a compound with the same molecular weight from LC-MS analysis and same retention time in HPLC analysis of the unknown impurity in TAEM was synthesized. |
| Key words：ceftazidine; TAEM; ceftazidine methyl |
|
作者簡(jiǎn)介： 厲 昆（1974-），男，浙江東陽(yáng)人，高級工程師，碩士研究生，主要從事醫藥中間體和藥物合成研究（E-mail：kun.li@apeloa.com）。
|
收稿日期：2014-11-24
|
|