反应 #2267065

ord-612187d51ba74addb6bf4bbb1d079fac

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他preheated to approximately 90° C., in separate 100-mL beakers
  2. 2
    workup.DISSOLUTIONto dissolve to a clear solution
  3. 3
    其他preheated to approximately 50° C.
  4. 4
    workup.ADDITIONwas added to the solution
  5. 5
    过滤The product was collected by vacuum filtration as white crystals
  6. 6
    其他to air dry

实验过程

Dimethyl sulfoxide (DMSO) was used as the primary solvent to solubilize Form I of 5-azacytidine and toluene was used as the co-solvent as follows. Approximately 250 mg of 5-azacytidine was dissolved with approximately 5 mL of DMSO, preheated to approximately 90° C., in separate 100-mL beakers. The solids were allowed to dissolve to a clear solution. Approximately 45 mL of toluene, preheated to approximately 50° C., was added to the solution and the resultant solution was mixed. The solution was covered and allowed to equilibrate at ambient conditions. The product was collected by vacuum filtration as white crystals using a Buchner funnel. The collected product was allowed to air dry.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06887855B2uspto-grants-2005_05