反应详情

To a solution of 3-nitro-phenol (143 mg, 1.03 mmol) in DMF (15 mL) was added sodium hydride (56 mg, 1.4 mmol) slowly and the mixture was stirred at rt for 30 min. 2-chloro-9-isopropyl-N-(1-methyl-1H-pyrazol-4-yl)-9H-purin-6-amine (200 mg, 0.69 mmol), as prepared in step 1 of Example 2, was added slowly. After the addition, the mixture was stirred at 110° C. overnight. The cooled reaction mixture was poured into water (100 mL) and extracted with EtOAc (2×30 mL). The combined organic extracts were dried over Na2SO4, concentrated and the residue was purified by flash column chromatography (MeOH:EtOAc=1:10) to give the title compound (50 mg, 18% yield) as light yellow oil.

1. additionwas added slowly
2. additionAfter the addition
3. stirringthe mixture was stirred at 110° C. overnight
4. customThe cooled reaction mixture
5. extractionextracted with EtOAc (2×30 mL)
6. dry with materialThe combined organic extracts were dried over Na2SO4
7. concentrationconcentrated
8. customthe residue was purified by flash column chromatography (MeOH:EtOAc=1:10)