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The preparation of 21-diazo-9 alpha-fluoro-16 alpha-methyl-21-deoxy-[1,2(n)-3H]prednisolone is described. [1,2(n)-3H]Dexamethasone 26 Ci/mmol, was oxidized with cupric acetate/air to give the 21-aldehyde. Treatment of the aldehyde with hydroxylamine gave the corresponding 21-oxime which was reacted with chloroamine to give a 25--35% yield of 21-diazo-9 alpha-fluoro-16 alpha-methyl-21-[1,2(n)-3H]deoxyprednisolone with a specific activity of 25--26 Ci/mmol.
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