Perchloric Acid → Florfenicol butyrate

HRID 507490

Reaktionsgleichung

Reaktionsgleichung von HRID 507490
[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)CCC)(=O)CCC>[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][CH2:9][CH3:10]

Komponenten

4

Edukt 2

HCID 24247Perchloric AcidHCID 114811Florfenicol

Produkt 1

HCID 131727111Florfenicol butyrate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7798Butyric anhydrideLösungsmittel

Versuchsvorschrift

225 g of florfenicol was suspended in 330 ml of butyric anhydride in one liter round bottom flask equipped with a over head stirrer and a drying tube. To this suspension was added one 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 florfenicol butyrate pro-drug was crystallized. The solid product was filtered using a Buckner funnel under vacuum, and washed thoroughly with hexane. The product was finally crystallized in ethanol and the crystallized product was washed with hexane and dried to obtain around 230 g of solid florfenicol butyrate.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-82ea8eaf7e6f422aaaad937db2a7df1b
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786167B2

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