Synthesis
Example 7 Synthesis of 1-amino-1,2,3-triazole (III)
813 mg of (1E,2E)-1,2-dihydrazinoethane (I) and 1.0 ml of ethanol were added to the reactor and mixed with stirring at room temperature. To the mixture was added 2.0 g of battery-grade manganese dioxide (Tosoh Corp. product; effective oxygen content ≥ 91%), kept at a constant temperature, and stirring was continued for 2 hours. Subsequently, another 1.0 g of battery grade manganese dioxide was added, the same temperature was maintained and stirring was continued for 5 hours. Upon completion of the reaction, the insoluble material was removed by filtration and the filtrate was concentrated under reduced pressure to give 720 mg (yield: 91%) of 1H-1,2,3-triazol-1-amine (III). The product was analyzed by 1H-NMR (DMSO-d6) and mass spectrometry (FAB+), and the m/e values, boiling point and melting point data were consistent with Example 1.
References
[1] Patent: US5728841, 1998, A
[2] Patent: US7550601, 2009, B1. Location in patent: Page/Page column 5
[3] Chinese Chemical Letters, 2014, vol. 25, # 2, p. 209 - 211
[4] Journal of Materials Chemistry, 2012, vol. 22, # 2, p. 666 - 674
