反応 #742274

ord-0084d7a7fafd4b9185f56e76aa32e93a

反応方程式

N[C@@H](C(=O)N[C@@H]1C(=O)N2C(C(=O)O)=C(Cl)CS[C@H]12)c1ccccc1
cefaclor
N[C@@H](C(=O)N[C@@H]1C(=O)N2C(C(=O)O)=C(Cl)CS[C@H]12)c1ccccc1
cefaclor
N
ammonia
N[C@@H](C(=O)N[C@@H]1C(=O)N2C(C(=O)O)=C(Cl)CS[C@H]12)c1ccccc1.O
cefaclor monohydrate

試薬

なし

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他30 min
  2. 2
    その他at 30° C.
  3. 3
    その他30 min
  4. 4
    その他at 25° C.
  5. 5
    その他60 min
  6. 6
    その他at 20° C
  7. 7
    ろ過The suspension was filtered through a glass
  8. 8
    ろ過filter
  9. 9
    洗浄the wet cake was washed with one volume of water and two volumes of acetone
  10. 10
    その他After drying

実験手順

A crystallisation reactor was filled with 34 g water and 1.0 g cefaclor as seed. The above-mentioned acidic cefaclor solution was dosed into the crystallisation reactor in 60 minutes at 35° C. The pH was kept at 5.0 with ammonia. Subsequently, the temperature was lowered in steps: 30 min at 30° C., 30 min at 25° C., and 60 min at 20° C. The suspension was filtered through a glass filter and the wet cake was washed with one volume of water and two volumes of acetone. After drying, 15.7 g cefaclor monohydrate was obtained (purity 99.4%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08071330B2uspto-grants-2011_12