反应详情

Triethyloxonium tetrafluoroborate (204 mg, 1.076 mmol) was added to a solution of the 4-{[2-chloro-3-(trifluoromethyl)phenyl]carbonyl}-2-piperazinone (I1)(300 mg, 0.978 mmol) in Dichloromethane (DCM) (6 mL) and the reaction was stirred for 1 h. To this was added the 3-hydroxy-2-pyridinecarbohydrazide (I93) (180 mg, 1.174 mmol) and the reaction was stirred for 2 hrs. The solvent was evaporated and 1-butanol (6.00 mL) was added. The mixture was heated at reflux for 3 h. After cooling the solvent was evaporated and the residue was partitioned between water/EtOAc. The organic layer was passed through a phase sep. cartridge and the solvent evaporated to afford an amber oil. This was purified by MDAP to afford a colourless solid of desired material in 90 mg.

1. stirringthe reaction was stirred for 2 hrs
2. customThe solvent was evaporated
3. addition1-butanol (6.00 mL) was added
4. temperatureThe mixture was heated
5. temperatureat reflux for 3 h
6. temperatureAfter cooling the solvent
7. customwas evaporated
8. customthe residue was partitioned between water/EtOAc
9. customcartridge and the solvent evaporated
10. customto afford an amber oil
11. customThis was purified by MDAP
12. customto afford a colourless solid of desired material in 90 mg