反应详情

温度

100 °C

2-acetyl-N-(3-bromopyridin-4-yl)hydrazinecarbothioamide (200 mg, 0.6917 mmol) was dissolved in sodium hydrogen carbonate (4 mL,) and stirred at 50° C. for 2 hrs and at 100° C. for 5 hrs. The reaction mixture was then allowed to stand at RT for 48 h before it was carefully neutralised with dilute HCl and partitioned with 10% MeOH in DCM. The aqueous layer was extracted with further 10% MeOH in DCM (3×10 mL) and the combined organics were dried over Na2SO4, filtered and concentrated under reduced pressure to give 4-(3-bromopyridin-4-yl)-5-methyl-4H-1,2,4-triazole-3-thiol as an orange solid (152.6 mg). MS (ES+) 272.9.

1. waitto stand at RT for 48 h before it
2. custompartitioned with 10% MeOH in DCM
3. extractionThe aqueous layer was extracted with further 10% MeOH in DCM (3×10 mL)
4. dry with materialthe combined organics were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure