Y. Tao
2013
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Journal
Fine chemicals
Abstract
A novel process of preparing 1H-tetrazole acetic acid is reported in this paper.Firstly,5-amino tetrazole was synthesized from hydrazine hydrate and cyanamide with a yield of 85%.Then,the intermediate was subjected to the second step of deamination reaction to give 1H-tetrazole with the yield of 95%.The last step was for 1H-tetrazole to go through nucleophilic substitution with chloroacetic acid.Under basic conditions,1H-tetrazole acetic acid was produced from 1H-tetrazole and chloroacetic acid with a yield of 81.7%.Water was used as the reaction medium in the above steps,and the total yield of 1H-tetrazole acetic acid was higher than 65%.The key focus of this paper was the optimization of nucleophilic substitution,and the optimum conditions were ascertained as follows:reaction temperature 100 ℃,n(1H-tetrazole)∶ n(ClCH2COOH)∶ n(NaHCO3)=1∶ 1∶ 2.2,reaction time 20 h.