تفاعل #59651

ord-ddc7ca042d31442d9c83c909303e04dd

معادلة التفاعل

C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23
levofloxacin
O=S([O-])S(=O)(=O)[O-].[Na+].[Na+]
sodium metabisulfite
C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23.C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23.O
levofloxacin hemihydrate

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةto reflux temperature
  3. 3
    workup.DISSOLUTIONuntil complete dissolution of the material
  4. 4
    ترشيحThe precipitate was filtrated under vacuum
  5. 5
    غسيلwashed with a mixture n-BuOH:H2O (9:1) (4 ml)
  6. 6
    أخرىdried at 60° C. in a vacuum oven

الإجراء التجريبي

1.5 g of levofloxacin crude and 10 mg of sodium metabisulfite were put in suspension in 6 ml of a mixture n-BuOH:H2O (9:1) under nitrogen atmosphere. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to RT over a period of 1.5 hours. The precipitate was filtrated under vacuum, washed with a mixture n-BuOH:H2O (9:1) (4 ml) and dried at 60° C. in a vacuum oven to give 1.2 g (81%) of purified levofloxacin hemihydrate. The purified levofloxacin hemihydrate contained virtually no N-oxide levofloxacin.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425628B2uspto-grants-2008_09