反应详情

To a solution of 4-[(2,4-dichloro-3-fluorophenyl)carbonyl]-2-piperazinone (I37) (0.364 g, 1.25 mmol) in Dichloromethane (DCM) (3 mL) was added triethyloxonium tetrafluoroborate (0.249 g, 1.313 mmol). The solution was then stirred, under argon, for 10 minutes before 4-pyrimidinecarbohydrazide (commercially available from e.g. Anichem, J&W PharmLab or Bepharm, 0.207 g, 1.500 mmol) was added. The solution was then stirred for a further hour before the solvent was concentrated and n-butanol (3.00 mL) was added. The solution was then stirred, under argon and reflux, for 3 hours before being cooled to room temperature. The solvent was then evaporated in vacuo and the remaining residue was purified by flash chromatography (Biotage SP4, 25M cartridge) with a gradient of 0-10% 2M NH3/MeOH in DCM. TLC confirmed product location and the solvent from the combined fractions were evaporated in vacuo. The remaining residue was then further purified by mass-direct automated HPLC, before the solvent was again evaporated in vacuo. The remaining solid was then triturated in ether before being dried in a vacuum oven to yield the product in 0.132 g.

1. additionwas added
2. concentrationwas concentrated
3. additionn-butanol (3.00 mL) was added
4. stirringThe solution was then stirred, under argon
5. temperaturereflux, for 3 hours
6. customThe solvent was then evaporated in vacuo
7. customthe remaining residue was purified by flash chromatography (Biotage SP4, 25M cartridge) with a gradient of 0-10% 2M NH3/MeOH in DCM
8. customthe solvent from the combined fractions were evaporated in vacuo
9. customThe remaining residue was then further purified by mass-direct automated HPLC, before the solvent
10. customwas again evaporated in vacuo
11. customThe remaining solid was then triturated in ether
12. custombefore being dried in a vacuum oven
13. customto yield the product in 0.132 g