反应详情

To a solution of 2-(n-propyl)amino-4-chloro-7-methyl-pyrrolo[2,3-d]pyrimidine (1.6 g, 7.1 mmol) in n-butanol (10 mL) was added potassium carbonate (4.9 g, 35.5 mmol), followed by propan-2-amine (632 mg, 10.7 mmol). The mixture was stirred in an autoclave equipped with a stirrer at 140° C. for 16 h. After cooling to room temperature, water was added (20 mL), and the mixture was extracted with EtOAc (3×50 mL). The combined organic layers were washed with water and then with a brine solution, and lastly dried over anhydrous Na2SO4. The volatiles were removed in vacuo and the residue was purified by flash column chromatography (PE/EtOAc=3/1) to yield 2-(n-propyl)amino-4-(i-propyl)amino-7-methyl-pyrrolo[2,3-d]pyrimidine (1.2 g, 75%) as a yellow solid. LCMS: (ESI) m/z=248 (M+H)+.

1. customequipped with a stirrer at 140° C. for 16 h
2. extractionthe mixture was extracted with EtOAc (3×50 mL)
3. washThe combined organic layers were washed with water
4. dry with materialwith a brine solution, and lastly dried over anhydrous Na2SO4
5. customThe volatiles were removed in vacuo
6. customthe residue was purified by flash column chromatography (PE/EtOAc=3/1)