2-(1H-1,2,4-triazol-3-yl)acetic acid hydrochloride synthesis

Yield:155049-60-8 50%

Reaction Conditions:

with methanol;sodium hydroxide;water in tetrahydrofuran at 100; for 2 h;

Steps:

15

Reference Example 15 1H-1,2,4-triazol-3-ylacetic acid A mixture of ethyl 1H-1,2,4-triazol-3-ylacetate obtained in Reference Example 14 (900 mg, 5.80 mmol), 4N aqueous sodium hydroxide solution (7.25 mL, 29.0 mmol), water (10 mL), methanol (10 mL) and THF (10 mL) was stirred at 100°C for 2 hr. The reaction mixture was concentrated under reduced pressure, the residue was acidified with 1N hydrochloric acid, and the mixture was concentrated under reduced pressure. Ethanol was added to the residue, and the insoluble material was filtered off, and the filtrate was concentrated. The residue was crystallized from toluene to give the title compound as a white powder (369 mg, 50%). ¹H-NMR (300MHz, DMSO-d₆) δ: 3.49 (2H, s), 7.92 (1H, s).

References:

EP1953148,2008,A1 Location in patent:Page/Page column 111