반응 #7302

ord-ad2378e8729f43cdb3501b2c8a8ba400

시약

없음

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to give 20 kg dispersion
  2. 2
    workup.DISSOLUTIONdissolved under ice-
  3. 3
    온도cooling
  4. 4
    기타to prepare a charge solution
  5. 5
    여과Thereafter, the solution was aseptically filtered through a 0.2 μm membrane
  6. 6
    여과filter (MCGL20S03, 0.2 μm, Millipore)
  7. 7
    기타equipped with a jacket)
  8. 8
    workup.STIRRINGThen, the crystallization tank was stirred
  9. 9
    기타by bubbling with nitrogen at 0 to 15° C.
  10. 10
    workup.ADDITION25 L isopropyl alcohol was aseptically added
  11. 11
    기타After crystallization, 55 L isopropyl alcohol
  12. 12
    workup.ADDITIONwas added aseptically
  13. 13
    workup.ADDITIONadded
  14. 14
    여과the precipitated crystals were collected aseptically by filtration
  15. 15
    세척The crystals were washed with isopropyl alcohol and acetone
  16. 16
    기타dried in a nitrogen stream with regulated humidity (20 to 40 RH %) for 10 hours or more

실험 절차

Water for injection was added to 2000 g titer equivalent amount of novel non-aseptic carbapenem hydrochloride derivative to give 20 kg dispersion. This dispersion was stirred and dissolved under ice-cooling to prepare a charge solution. Thereafter, the solution was aseptically filtered through a 0.2 μm membrane filter (MCGL20S03, 0.2 μm, Millipore) and fed to a crystallization tank (equipped with a jacket). Then, the crystallization tank was stirred by bubbling with nitrogen at 0 to 15° C., and 25 L isopropyl alcohol was aseptically added thereto. After crystallization, 55 L isopropyl alcohol was added aseptically added thereto over 1 hour or so. After aging for a predetermined time, the precipitated crystals were collected aseptically by filtration. The crystals were washed with isopropyl alcohol and acetone, and dried in a nitrogen stream with regulated humidity (20 to 40 RH %) for 10 hours or more, to give novel aseptic carbapenem hydrochloride trihydrate crystals.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084268B1uspto-grants-2006_08