反应详情

To a solution of N2-(2,3-dimethyl-2H-indazol-6-yl)-5-methyl-N4-(3-azaspiro[5.5]undecan-9-yl)pyrimidine-2,4-diamine (201.5 mg, 0.4802 mmol), HOAT (106.4 mg, 0.7817 mmol) and EDCI (145.7 mg, 0.7600 mmol) in DCM/DMF (4 mL/1 mL) were added N,N-diethylethanamine (207.6 mg, 2.052 mmol) and acetic acid (36.7 mg, 0.611 mmol). The reaction was stirred at rt for 2 h. The reaction solution was concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=30/1) to give the crude product as a light yellow solid (92 mg). The crude product was recrystallized from acetone/MeOH (6 mL/0.5 mL) to give the title compound as a white solid (50.4 mg, 21.6%).

1. concentrationThe reaction solution was concentrated in vacuo
2. customThe residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=30/1)
3. customto give the crude product as a light yellow solid (92 mg)
4. customThe crude product was recrystallized from acetone/MeOH (6 mL/0.5 mL)