反应详情

A mixture of 1 (250 mg, 0.59 mmol) and 4H-[1,2,4]Triazole-3,5-diamine (58.91 mg, 0.59 mmol) in acetic acid (0.4 mL) and ethanol (1.6 mL) was heated under reflux for 6 hours. After cooling, the mixture was diluted with 15 mL of DCM, the combined organic phase was washed with NaHCO3 aq. and brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by prep.TLC to give 6-1. MS (ESI) m/e (M+H+) 457.3

1. temperaturewas heated
2. temperatureunder reflux for 6 hours
3. temperatureAfter cooling
4. washthe combined organic phase was washed with NaHCO3 aq. and brine
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated
7. customThe residue was purified by prep.TLC
8. customto give 6-1