Yield:3641-14-3 65%

Reaction Conditions:

with thionyl chloride at 70; for 48 h;

Steps:

7.3 Methyl 5-amino-1H-1,2,4-triazole-3-carboxylate
To a solution of 5-amino-lH-l ,2,4-triazole-3-carboxylic acid (3.9 g, 30.45 mmol) in methanol (100 ml) was added SOCl₂ (12 g, 100.84 mmol). The resulting solution was stirred for 48 h at 70°C. The resulting mixture was concentrated under vacuum, dissolved in water (100 ml), the H was adjusted to 8 with NaHCC>3 solution, and then extracted with dichloromethane (3 x 50 ml). The organic layer was dried over anhydrous magnesium sulfate and concentrated under vacuum to afford methyl 5- amino-lH-l ,2,4-triazole-3-carboxylate as a white solid (800 mg, 65%). LC/MS (ES, m/z): [M+H]⁺ 143.0 *H NMR (300 MHz, DMSO): δ, 3.85 (s, 3H)

References:

BIOENERGENIX;MCCALL, John;KELLY, Robert, C.;ROMERO, Donna, L WO2014/66743, 2014, A1 Location in patent:Paragraph 0146

FullText