반응 #59654

ord-5ef30b4014b14c6b9ef8a9cf7daa197a

반응 방정식

C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23
levofloxacin
→
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
수율 84.0%

반응물

C[C@H]1COc2c(N3CCN(C)CC3)c(F)cc3c(=O)c(C(=O)O)cn1c23
levofloxacin

시약

없음

용매

CCC(C)=O
MEK

반응 조건

온도
-5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    온도to reflux temperature
  3. 3
    workup.DISSOLUTIONuntil complete dissolution of the material
  4. 4
    여과The precipitate was filtrated under vacuum
  5. 5
    세척washed with 1.5 ml of MEK
  6. 6
    기타dried at 30° C. in a vacuum oven

실험 절차

1.5 g of levofloxacin crude was put in suspension in 15 ml of MEK. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to −5° C. over a period of 3 hours. The precipitate was filtrated under vacuum, washed with 1.5 ml of MEK and dried at 30° C. in a vacuum oven to give 840 mg (84%) of purified levofloxacin hemihydrate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07425628B2uspto-grants-2008_09