1,3,4-Oxadiazole-2-MethanaMine, hydrochloride synthesis

Yield:1383788-35-9 88.7%

Reaction Conditions:

with hydrogenchloride in ethyl acetate at 0 - 20; for 16 h;

Steps:

2S-I-4.4 Synthesis of (1, 3, 4-oxadiazol-2-yl) methanamine (2S-U)

To a stirring solution of 2S-T (5 g, 25 mmol) in EtOAc (10 mL) was added EtOAc saturated with HC1 (60 mL) at 0 °C and stirred at RT for 16 h. After consumption of the starting material (by TLC), the reaction mixture was concentrated under reduced pressure. The crude material was triturated with diethylether/w-pentane (25 mL/25 mL) and dried under reduced pressure to afford 2S-U (3 g, 88.7%) as an off-white solid (HC1 salt). XH-NMR: (500 MHz, DMSO-i): δ 9.55 (br s, 2H), 7.99 (s, 1H), 3.90 (s, 2H); LCMS m/z: 100 [M⁺+l]

References:

WO2014/120783,2014,A1 Location in patent:Paragraph 00139