Reacción #162784
ord-2f5bd3442d214e6f991724730827f825
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Otrothen partitioned between EtOAc and water
- 2ExtracciónThe aqueous layer was then extracted with EtOAc (3×)
- 3LavadoThe combined organic layers were washed with brine
- 4Secadodried (MgSO4)
- 5Filtraciónfiltered
- 6Otroevaporated in vacuo
- 7OtroThe residue was purified by FCC
Procedimiento
Triisopropylsilylchloride (1.02 mL, 3.96 mmol) was added to a solution of 3-(5-amino-3-tert-butyl-pyrazol-1-yl)-phenol (915 mg, 3.96 mmol) and imidazole (646 mg, 9.50 mmol) in DMF (15 mL) at 0° C. The reaction was stirred at RT over the weekend then partitioned between EtOAc and water. The aqueous layer was then extracted with EtOAc (3×). The combined organic layers were washed with brine, dried (MgSO4), filtered and evaporated in vacuo. The residue was purified by FCC, using 0-40% EtOAc in cyclohexane, to give the title compound (1.53 g, 99%). LCMS (Method 4): Rt 4.78 min, m/z 388 [MH+].