反应详情

To a suspension of CDI (17.24 g, 106 mmol) in DCM (150 mL) was added 3-tert-butyl-1-p-tolyl-1H-pyrazol-5-amine (24.38 g, 106 mmol) in 1 g portions over 40 min and the reaction stirred at RT for 2 hr. An aliquot of this solution (5.0 mL,) was added dropwise to a suspension of 4-(4-aminonaphthalen-1-yloxy)pyrimidin-2-amine (720 mg, 2.85 mmol) in DCM (15 mL) and the mixture maintained at RT for 2 hr. The reaction mixture was diluted with DCM (20 mL) and was washed with water (30 mL) and brine (30 mL) and then dried (MgSO4) and evaporated in vacuo. The residue was purified by flash column chromatography (SiO2, EtOAc in isohexane, 20-60%, gradient elution) to afford the title compound, Intermediate P1, as a beige solid (1.21 g, 83%); Rt 2.12 min (Method 2); m/z 508 (M+H)+, (ES+)+.

1. temperaturethe mixture maintained at RT for 2 hr
2. washwas washed with water (30 mL) and brine (30 mL)
3. dry with materialdried (MgSO4)
4. customevaporated in vacuo
5. customThe residue was purified by flash column chromatography (SiO2, EtOAc in isohexane, 20-60%, gradient elution)