第 38 卷第 4 期 | ![](image2/wentou.gif) | Vol. 38 No. 4 | 2008 年 8 月 | Aug 2008 |
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所属栏目:有机合成原料
N,N ′-二叔丁氧基羰基-1H-吡唑-1-甲脒的合成 |
黄长江,袁 静,徐为人,王平保
(天津药物研究院,天津 300193) |
摘 要:1H-吡唑-1-甲脒盐酸盐在碳酸钾存在下和二碳酸二叔丁酯反应制备了N-叔丁氧基羰基-1H-吡唑-1-甲脒(PB),PB和二碳酸二叔丁酯在4-二甲氨基吡啶的催化下反应制备了N,N,N′-三叔丁氧基羰基-1H-吡唑-1-甲脒(PT),PT和高氯酸镁六水合物反应制备了标题化合物。反应条件温和,总收率65.9%,产品纯度大于99.0%,产品结构经熔点、核磁和质谱确定。 |
关键词:胍;1H-吡唑-1-甲脒;二碳酸二叔丁酯;N,N′-二叔丁氧基羰基-1H-吡唑-1-甲脒;合成 |
中图分类号:O626.21 文献标识码:A 文章编号:1009-9212(2008)04- 0041-03 |
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Synthesis of N,N′-di-Boc-1H-pyrazole-1-carboxamidine |
HUANG Chang-jiang,YUAN Jing,XU Wei-ren,WANG Ping-bao
(Tianjin Institute of Pharmacentical Research,Tianjin 300193,China) |
Abstract:N,N′-di-Boc-1H-pyrazole-1-carboxamidine was synthesized from 1H-pyrazole-1-carboxamidine hydrochloride(PJ). PJ was treated with di-tert-butyl dicarbonate in the presence of K2CO3 to give N-Boc-1H-pyrazole-1-carboxamidine(PB),then PB reacted with di-tert-butyl dicarbonate in the presence of 4-dimethylaminopyridine to give N,N,N′-tri-Boc-1H-pyrazole-1-carboxamidine(PT),PT reacted with Mg(ClO4)·6H2O to give N,N'-di-Boc-1H-pyrazole-1-carboxamidine(PM). The overall yield and the purity product was 65.9% and 99.0%,respectively. The structure of the product was identified by m.p.,1H NMR and MS. |
Key words:guanidine;1H-pyrazole-1-carboxamidine;di-tert-butyl dicarbonate;N,N′-di-Boc-1H-pyrazole-1-carboxamidine;synthesis |
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作者简介: 黄长江(1977-),男,河北唐山人,硕士,助理研究员,主要从事有机合成和新药研发。(E-mial:xiaohuo3@yahoo.com.cn)
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收稿日期:2008-07-15
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