Improved synthesis of dipyridyl thioselenosemicarbazones
10.13220/j.cnki.jipr.2016.03.015
- Author:
Xiao-Dong XING
1
Author Information
1. Institute of Pharmacology and Toxicology, Academy of Military Medical Sciences
- Publication Type:Journal Article
- Keywords:
Dipyridyl thioselenosemicarbazones;
Metal-chelator;
Process improvement;
Synthesis
- From:
Journal of International Pharmaceutical Research
2016;43(3):481-484
- CountryChina
- Language:Chinese
-
Abstract:
Objective To improve the synthesis process of N- allyl- 2-(di(pyridin- 2- yl)methylene)hydrazinecarboselenoamide(4)and2-(di(pyridin-2-yl)methylene)-N,N-dimethylhydrazinecarboselenoamide(8). Methods 4-allyl-3-thiosemicarbazide (1)was the starting material,which reacted with methyl iodide,sodium hydrogen selenide to obtain intermediate 4-allyl-3-selenosemicarbazide(3). Compound(3)reacted with di-2-pyridyl ketone to obtain the target compound 4. 4,4-Dimethyl-3-thiosemicarbazide was the starting materials,which reacted with di-2-pyridyl ketone to obtain intermediate dipyridyl thiosemicarbazone(6). Compound 6 reacted with methyl iodide,sodium hydrogen selenide to obtain the target compound 8. We optimized the reaction conditions of each step. Results We synthesized the target compound 4 and 8 according to the respective synthetic route,the structure of the target compounds and the intermediates were confirmed by 1H NMR and MS. Conclusion The improved processes are easy to operate,cost-saving and suitable for large scale preparation.
