反应详情

Triethyloxonium tetrafluoroborate (197 mg, 1.039 mmol) was added to a solution of the 4-[(2,3-dichloro-4-fluorophenyl)carbonyl]-2-piperazinone (I34) (275 mg, 0.945 mmol) in Dichloromethane (DCM) (6 mL) and the reaction was stirred for 1 h. To this was added the 5-methyl-2-furancarbohydrazide (I85) (159 mg, 1.134 mmol) and the reaction was stirred for 2 h. The solvent was evaporated and 1-butanol (6.00 mL) was added. The mixture was heated at reflux for 3 h. LCMS: Product peak observed. After cooling the solvent was evaporated and the residue was partitioned between water/EtOAc. The organic layer was dried (Na2SO4) and the solvent evaporated to afford a brown oil. This was purified by MDAP to afford a colourless solid of desired material in 38 mg.

1. stirringthe reaction was stirred for 2 h
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. dry with materialThe organic layer was dried (Na2SO4)
10. customthe solvent evaporated
11. customto afford a brown oil
12. customThis was purified by MDAP
13. customto afford a colourless solid of desired material in 38 mg