HCID 131725880, compound → HCID 131725879, compound
Reaction equation
[ClH:1].[CH2:2]1[C@@H:6]2[CH2:7][C:8](=[O:9])[N:5]2[CH:4]=[CH:3]1>O>[OH2:9].[OH2:9].[OH2:9].[ClH:1].[CH2:2]1[C@@H:6]2[CH2:7][C:8](=[O:9])[N:5]2[CH:4]=[CH:3]1Participants
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
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.
Workup
- customto give 20 kg dispersion
- dissolutiondissolved under ice-
- temperaturecooling
- customto prepare a charge solution
- filtrationThereafter, the solution was aseptically filtered through a 0.2 μm membrane
- filtrationfilter (MCGL20S03, 0.2 μm, Millipore)
- customequipped with a jacket)
- stirringThen, the crystallization tank was stirred
- customby bubbling with nitrogen at 0 to 15° C.
- addition25 L isopropyl alcohol was aseptically added
- customAfter crystallization, 55 L isopropyl alcohol
- additionwas added aseptically
- additionadded
- filtrationthe precipitated crystals were collected aseptically by filtration
- washThe crystals were washed with isopropyl alcohol and acetone
- customdried in a nitrogen stream with regulated humidity (20 to 40 RH %) for 10 hours or more
Sources & evidence
- ORD record
- ord-ad2378e8729f43cdb3501b2c8a8ba400
- Source dataset
- uspto-grants-2006_08
- Patent number
- US07084268B1
Reaction notes
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