反应详情

To a solution of diethyl 4-((6-amino-2-(2-methoxyethoxy)-9H-purin-9-yl)methyl)benzylphosphonate (1 equiv.) in acetic acid (0.20 M) was added sodium acetate (15 equiv.) and bromine (13 equiv.). The reaction mixture was then allowed to stir at room temperature for 18 h. At this point the reaction was quenched by the addition of sodium thiosulfate. The mixture was then diluted with water and DCM. This mixture was transferred to a separatory funnel and washed with DCM three times. The combined organic layers were then dried over anhydrous Na2SO4 and the volatiles were removed in vacuo. The resulting residue was purified by a COMBIFLASH™ system using a gradient of 0-5% MeOH/DCM to provide the title compound (14%) as a solid.

1. customAt this point the reaction was quenched by the addition of sodium thiosulfate
2. additionThe mixture was then diluted with water and DCM
3. customThis mixture was transferred to a separatory funnel
4. washwashed with DCM three times
5. dry with materialThe combined organic layers were then dried over anhydrous Na2SO4
6. customthe volatiles were removed in vacuo
7. customThe resulting residue was purified by a COMBIFLASH™ system