反应详情

温度

50 °C

To a solution of 6-{6-[1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazol-4-yl]-[1,2,4]triazolo[4,3-b]pyridazin-3-ylsulfanyl}-quinoline (150 mg, 0.32 mmol) in dichloromethane (8 mL) at 0° C. was added trifluoroacetic acid. After 3 hours the mixture was concentrated to dryness and taken Up in dichloromethane and neutralized via the addition of aqueous NaHCO3. To this emulsion was added a chloroform/methanol (95/5) mixture (20 mL) and brine (30 mL). The organic phase was separated and the organic phase filtered and the solid residue washed with water then Et2O and dried to return a yellow solid (64 mg). This solid was taken up in methanol (2 mL) to which ethylenediamine (1 mmol) was added and heated at 50° C. for 1 hour. The mixture was cooled to ambient temperature and the solid collected via filtration and dried to return title compound as a white solid (57 mg, 0.17 mmol, 53% yield).

1. concentrationAfter 3 hours the mixture was concentrated to dryness
2. additiontaken Up in dichloromethane and neutralized via the addition of aqueous NaHCO3
3. additionTo this emulsion was added a chloroform/methanol (95/5) mixture (20 mL) and brine (30 mL)
4. customThe organic phase was separated
5. filtrationthe organic phase filtered
6. washthe solid residue washed with water
7. dry with materialEt2O and dried
8. additionwas added
9. temperatureThe mixture was cooled to ambient temperature
10. filtrationthe solid collected via filtration
11. customdried