5 Aminotetrazole Monohydrate Lab Report

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5-aminotetrazole monohydrate: In a 250 ml round-bottom flask equipped with a condenser for refluxing (90 °C) and a magnetic stirring bar, 5.00 g (5.95 mmol) dicyandiamide (three times crystallized), 7.47 g (11.9 mmol) sodium azide and 11.00 g (17.8 mmol) boric acid and 100 ml of water is added and allowed to reflux for 24 hours, after the completion of the reaction, until the solution pH to about 2 to 3 as hydrochloric acid 37% is added (about 12 ml) Then the reaction mixture was cooled in a refrigerator for 18 hours and the white crystals formed. The mixture was filtered and washed three times with 10 ml of water and and dried in 60 °C for 5 hours and finally 45.8 g of product by it will be obtained. 5-Aminotetrazol monohydrate: Yield:,…show more content…
Chloroacetic acid (0.5 g, 5. 28 mmol), 5-aminotetrazole monohydrate (0.45 g, 5. 28 mmol), and sodium hydroxide (0.59 g, 10.57 mmol) in 10 ml of water was refluxed 20 hr, cooled, and made strongly acidic with concentrated hydrochloric acid. The mixture was cooled overnight and precipitate was separated to give 0.28 g a white solid product at 45.41% yield. (5-Amino-tetrazol-1-yl)-acetic acid: Yield: 45.41%; white crystals; m.p 210-213°C; IR (KBr): 3388, 3315, 3270, 3205, 3010, 2976, 1697, 1638, 1586, 1496, 1257 cm-1; 13C NMR (75 MHz (DMSO-d6)): 168, 156,…show more content…
N-(1-Carboxymethyl-1H-tetrazol-5-yl)-hydrazinium nitrate (3). A solution of AgNO3 (0.10 g, 0.60 mmol) in distilled water (1.5 mL) was added dropwise in the dark to the solution of compound 2 (0.10 g, 0.60 mmol) in Deionized water (1.5 mL) under stirring. After 2-3 hour, the precipitate was filtered, and rinsed with 4 mL distilled water. The solvent was removed by rotary Evaporation to produce a white solid at 88% yield (0.10 g); N-(1-Carboxymethyl-1H-tetrazol-5-yl)-hydrazinium nitrate: Yield: 88%; yellow crystals;. IR (KBr): 3396, 3329, 3140, 3008, 1628, 1494, 1383 cm-1; UV (H2O): λmax = 293-296

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