反应详情

温度

50 °C

To a stirred suspension of 6-chloropurine (5.0 g, 29.48 mmol) and K2CO3 (4.48 g, 32.42 mmol) in dry DMF 1-bromo-3-chloropropane (13.92 g, 88.45 mmol) is added. The reaction mixture is heated to 50° C. for 1 min and stirred at room temperature for additional 3 h. The reaction mixture is poured into 120 mL of water and extracted with CH2Cl2. The combined organic phases are washed with water, dried over MgSO4 and evaporated in vacuo. The residue is purified by flash column chromatography (dichloromethane/methanol 50:1 to 10:1) to yield 2.6 g (10.65 mmol, 35%) of the title compound as a colorless solid. 1H-NMR (400 MHz, DMSO-d6): δ=8.11 (s, 1H, H-8), 6.91 (s, 2H, NH2), 4.16 (t, J=6.8, 2H, CH2), 3.63 (t, J=6.8, 2H CH2), 2.25 (m, 2H, CH2) ppm. MS (ESI) m/z 247.3 [M+H]+.

1. additionis added
2. extractionextracted with CH2Cl2
3. washThe combined organic phases are washed with water
4. dry with materialdried over MgSO4
5. customevaporated in vacuo
6. customThe residue is purified by flash column chromatography (dichloromethane/methanol 50:1 to 10:1)