The general procedure for the synthesis of 2H-2-acetic acid-1,2,3-triazole-1,2,3-triazole from ethyl 2-(2H-1,2,3-triazol-2-yl)acetate was as follows:
1. Preparation of 2H-1,2,3-triazol-2-ylacetic acid: a solution of lithium hydroxide monohydrate (2.5 g, 60 mmol) in water (15 mL) was added to a solution of ethyl 2-(2H-1,2,3-triazol-2-yl)acetate (7.8 g, 50 mmol), and the reaction was stirred for 18 h at room temperature.
2. Upon completion of the reaction, the reaction mixture was acidified with 2M hydrochloric acid (150 mL) followed by extraction with dichloromethane (150 mL x 3).
3. The organic phases were combined, dried over magnesium sulfate and concentrated under reduced pressure to afford 2H-2-acetic acid-1,2,3-triazole as a white solid in 81% (5.2 g) yield. 4.
4. Product characterization: 1H NMR (400 MHz, CDCl3) δ: 5.35 (s, 2H), 7.72 (s, 2H); LRMS APCI m/z 128 [M + H]+.
