Moxifloxacin hydrochloride monohydrate → Moxifloxacin hydrochloride

HRID 882994Notes

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]

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

  1. customequipped with a mechanical stirrer
  2. temperaturereflux condenser
  3. temperatureto reflux
  4. customwas then reduced to 20° C.
  5. filtrationthe solid was filtered out
  6. washwashed with 900 ml of absolute ethanol
  7. customdried under vacuum (30 mmHg) at 40° C. for 18 hours

Sources & evidence

ORD record
ord-debf542b66d647248987757ccc77b984
Source dataset
uspto-grants-2012_08
Patent number
US08236817B2

Reaction notes

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