反应详情

A solution of 6-chloro-N′-methylnicotinimidohydrazide (2BX) (2.4 g, 13 mmol) in Formic Acid (99%, 10 ml) was stirred at reflux temperature for 1 hour. Reaction was cooled and solvent evaporated. The residue was extracted with EtOAc (100 ml) and Aqueous NaHCO3 (50 ml), organic layer was separated, dried over Na2SO4, filtered and solvent evaporated. The residue chromatographed on silica gel eluting with 10% MeOH:CH2Cl2 yielding title product as a solid (1.8 g, 72%) MS (MH, 195)

1. temperatureat reflux temperature for 1 hour
2. customReaction
3. temperaturewas cooled
4. customsolvent evaporated
5. extractionThe residue was extracted with EtOAc (100 ml) and Aqueous NaHCO3 (50 ml), organic layer
6. customwas separated
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customsolvent evaporated
10. customThe residue chromatographed on silica gel eluting with 10% MeOH