西索米星

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 15 g of the pure sisomicin base are dissolved in 60 ml of ion free water and to that solution as much 5 N sulfuric acid solution is added dropwise, as in needed to obtain a level of pH 4.3. Thereafter 1.5 g of active charcoal are added to the solution and the mixture is stirred for 30 minutes, then filtered on Seitz sheet. The filter is washed with 3×50 ml of ion free water and the unified filtrate is added by continuous stirring to 1 liter of methanol. The solution containing separated precipitate is allowed to stand in a cooling room, whereafter the precipitate is filtered out. The filtered sisomicin sulfate is washed with 3×50 ml of methanol, and dried in vacuum at 50° C. above P2O5 to constant weight. Thus 22 g of sisomicin sulfate are obtained. is added dropwise to obtain a level of pH 4.3 filtered on Seitz sheet The filter is washed with 3×50 ml of ion free water the unified filtrate is added by continuous stirring to 1 liter of methanol The solution containing separated precipitate is filtered out The filtered sisomicin sulfate is washed with 3×50 ml of methanol dried in vacuum at 50° C. above P2O5 to constant weight

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: in the procedure of above Example 1A instead of adding 1 N sulfuric acid to the solution of sisomicin in water until it reaches a pH of about 5, other acids may be used, such as acetic acid, trifluoroacetic acid, p-toluenesulfonic acid, hydrochloric acid, phosphoric acid, or nitric acid. The acidified aqueous solution is then treated with acetaldehyde and sodium cyanoborohydride and the resultant product is purified as described above, whereby is obtained 1-N-ethylsisomicin. the resultant product is purified