反应详情

The product of Example 5, Step 2 (0.100 g, 0.330 mmol, 1.00 equiv), 3-chloro-1H-indazol-5-amine (84 mg, 0.502 mmol, 1.50 equiv) and PS-carbodiimide resin (456 mg, 0.502 mmol, 1.00 equiv) were suspended in 2.0 mL DMF and stirred overnight at room temperature. The reaction mixture was concentrated to approximately 1 mL DMF and water was added. The resulting precipitate was collected by filtration and washed with 50% CH2Cl2/hexanes. The product was purified by preparative reverse phase HPLC (19×50 Xterra Prep RP 10-90% CH3CN/5 mM NH4HCO3 over 9 min, 25 ml/min) to provide 5.0 mg (3%) of the title compound as a white solid. MS (ES+) m/e 449 [M+H]+

1. concentrationThe reaction mixture was concentrated to approximately 1 mL DMF and water
2. additionwas added
3. filtrationThe resulting precipitate was collected by filtration
4. washwashed with 50% CH2Cl2/hexanes
5. customThe product was purified by preparative reverse phase HPLC (19×50 Xterra Prep RP 10-90% CH3CN/5 mM NH4HCO3 over 9 min, 25 ml/min)