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Moxifloxacin hydrochloride monohydrate → Moxifloxacin Hydrochloride

HRID 882994
Notes
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Reaction equation

HRID 882994 reaction equation
[CH3:1][O:2][C:3]1[C:8]([N:9]2[CH2:17][C@@H:16]3[C@@H:11]([CH2:12][CH2:13][CH2:14][NH:15]3)[CH2:10]2)=[C:7]([F:18])[CH:6]=[C:5]2[C:19]([C:21]([C:27]([OH:29])=[O:28])=[CH:22][N:23]([CH:24]3[CH2:26][CH2:25]3)[C:4]=12)=[O:20].O.[ClH:31]>C(O)C>[CH3:1][O:2][C:3]1[C:8]([N:9]2[CH2:17][C@@H:16]3[C@@H:11]([CH2:12][CH2:13][CH2:14][NH:15]3)[CH2:10]2)=[C:7]([F:18])[CH:6]=[C:5]2[C:19]([C:21]([C:27]([OH:29])=[O:28])=[CH:22][N:23]([CH:24]3[CH2:26][CH2:25]3)[C:4]=12)=[O:20].[ClH:31]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

HCID 9890250Moxifloxacin hydrochloride monohydrate

Product 1

HCID 101526Moxifloxacin Hydrochloride

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

907.4 g of moxifloxacin hydrochloride monohydrate and 9070 ml of absolute ethanol (K.F.<0.1%) were failed into a 10 liter jacketed reactor and equipped with a mechanical stirrer, reflux condenser, and thermometer. The suspension was brought to reflux with stirring and was kept in those conditions for 4 hours. The temperature was then reduced to 20° C. and the solid was filtered out and washed with 900 ml of absolute ethanol. The filtered solid was then discharged and dried under vacuum (30 mmHg) at 40° C. for 18 hours to give moxifloxacin hydrochloride form A having a water content of about 1% K.F.).

Workup

  • customequipped with a mechanical stirrer
  • temperaturereflux condenser
  • temperatureto reflux
  • customwas then reduced to 20° C.
  • filtrationthe solid was filtered out
  • washwashed with 900 ml of absolute ethanol
  • customdried under vacuum (30 mmHg) at 40° C. for 18 hours
  • Sources & evidence

    ORD record
    ord-debf542b66d647248987757ccc77b984
    Source dataset
    uspto-grants-2012_08
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US08236817B2

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes