反应详情

To a solution of 4-amino-1,2,5-oxadiazole-3-carboxylic acid (0.25 g, 1.9 mmol) in 2 mL of EtOH was added SOCl2 (0.2 mL) dropwise, under cooling with an ice-bath. The resulting mixture was refluxed for 4 hours and then concentrated. The oil was diluted with 50 mL of H2O and extracted with diethyl ether (3×100 mL). The combined organic layer was dried over MgSO4 and concentrated to give a white solid (0.15 g, 50%). 1H NMR (DMSO, 500 MHz) δ 6.39 (s, 2H), 4.39 (q, 2H), 1.35 (t, 3H). Mass Spec. FIA MS 158.1 (M+1).

1. temperatureunder cooling with an ice-bath
2. temperatureThe resulting mixture was refluxed for 4 hours
3. concentrationconcentrated
4. additionThe oil was diluted with 50 mL of H2O
5. extractionextracted with diethyl ether (3×100 mL)
6. dry with materialThe combined organic layer was dried over MgSO4
7. concentrationconcentrated