反应详情

To a stirred solution of 9-benzylpurine (6) (15.0 g, 66.5 mmol) in chloroform (750 mL) was added N-bromosuccinimide (59.26 g, 332.9 mmol) and the reaction mixture was stirred under an atmosphere of nitrogen at reflux temperature for 3 h. The reaction mixture was then transferred to a separatory funnel and washed with saturated aqueous sodium sulfite (2×250 mL) followed by brine solution (2×250 mL). The chloroform fraction was dried over anhydrous sodium sulfate and concentrated to give a reddish oil, which was purified by flash chromatography on silica gel using EtOAc/hexane (4:6) for elution. Yield 9.72 g. (48%). Mp 199-201° C. 1H NMR (CDCl3) δ 5.39 (s, 2H, benzylic CH2), 7.29-7.33 (m, 5H, Ar—H), 8.29 (s, 1H, purine C2—H).

1. temperatureat reflux temperature for 3 h
2. customThe reaction mixture was then transferred to a separatory funnel
3. washwashed with saturated aqueous sodium sulfite (2×250 mL)
4. dry with materialThe chloroform fraction was dried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customto give a reddish oil, which
7. customwas purified by flash chromatography on silica gel
8. washfor elution