反应详情

A mixture of 1.81 g of 2-hydroxymethyl-3H-imidazo[5,4-d]pyrimidine (prepared as described in Preparation 48), 2.71 g of t-butyldimethylsilyl chloride, 2.45 g of imidazole and 100 ml of dimethylformamide was stirred at room temperature for 1 hour. At the end of this time, the reaction mixture was freed from dimethylformamide by distillation under reduced pressure. The residue thus obtained was diluted with water, after which it was extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, after which the solvent was removed by distillation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, using ethyl acetate as the eluent, to give 1.89 g of the title compound, melting at 104°-107° C.

1. distillationAt the end of this time, the reaction mixture was freed from dimethylformamide by distillation under reduced pressure
2. customThe residue thus obtained
3. extractionafter which it was extracted with ethyl acetate
4. washThe extract was washed with an aqueous solution of sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. customafter which the solvent was removed by distillation under reduced pressure
7. customThe resulting residue was purified by column chromatography through silica gel