反应详情

A 0.3 M aqueous solution of NaNO2 (200 mL, 60 mmol) was added dropwise to a cooled (−15° C.), vigorously stirred suspension of 2-amino-6-chloro-9H-purine (6.0 g, 35.4 mmol) in 120 mL HBF4 (48 w % in H20, 0.92 mol) over 75 min. The pale yellow reaction was stirred at r. t. for 20 min and then recooled to −15° C. and neutralized to PH=6.0 with aqueous NaOH (50 w % in H2O). The water was removed in vacuo and the resulting orange solid chromatographed on silica gel (90:10 CH2Cl2:MeOH, Rf 0.50). The final product was obtained as white solid (3.0 g, 49.1%).

1. temperaturea cooled
2. customThe pale yellow reaction
3. customThe water was removed in vacuo
4. customthe resulting orange solid chromatographed on silica gel (90:10 CH2Cl2:MeOH, Rf 0.50)