Perchloric Acid → Florfenicol hexanoate

HRID 507492

Reaktionsgleichung

Reaktionsgleichung von HRID 507492
[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C@@H:11]([OH:21])[C@H:12]([NH:15][C:16]([CH:18]([Cl:20])[Cl:19])=[O:17])[CH2:13][F:14])=[CH:9][CH:10]=1)(=[O:4])=[O:3].Cl(O)(=O)(=O)=[O:23]>C(OC(=O)CCCCC)(=O)CCCCC>[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C@@H:11]([OH:21])[C@H:12]([NH:15][C:16]([CH:18]([Cl:20])[Cl:19])=[O:17])[CH2:13][F:14])=[CH:9][CH:10]=1)(=[O:4])=[O:3].[C:11]([O-:21])(=[O:23])[CH2:8][CH2:7][CH2:6][CH2:5][CH3:10]

Komponenten

4

Edukt 2

HCID 24247Perchloric AcidHCID 114811Florfenicol

Produkt 1

HCID 86596088Florfenicol hexanoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 74918Hexanoic anhydrideLösungsmittel

Versuchsvorschrift

100 g of florfenicol was suspended in 500 g of hexanoic anhydride in one liter round bottom flask equipped with an overhead stirrer and a drying tube. To this suspension was added 3 ml of perchloric acid, while stirring vigorously, with a pipette. A clear solution was obtained in a few minutes. Stirring was continued for another 3 hours during which the product, florfenicol hexanoate pro-drug was recrystallized. The solid product was filtered using Buckner funnel under vacuum, washed thoroughly with hexane. The product was finally recrystallized in ethanol and the recrystallized product was washed with hexane and dried to obtain around 117 g of solid florfenicol hexanoate.

Aufarbeitung

  1. customequipped with an overhead stirrer and a drying tube
  2. customA clear solution was obtained in a few minutes
  3. stirringStirring
  4. customthe product, florfenicol hexanoate pro-drug was recrystallized
  5. filtrationThe solid product was filtered
  6. washwashed thoroughly with hexane
  7. customThe product was finally recrystallized in ethanol
  8. washthe recrystallized product was washed with hexane
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-544ae32c5ab54aa887c6cd44ba6839af
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786167B2

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