Perchloric Acid → HCID 86596087, Verbindung

HRID 507491

Reaktionsgleichung

Reaktionsgleichung von HRID 507491
[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)C)(=O)C>[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:16]([O-:23])(=[O:17])[CH3:18]

Komponenten

4

Edukt 2

HCID 24247Perchloric AcidHCID 114811Florfenicol

Produkt 1

HCID 86596087HCID 86596087, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7918Acetic AnhydrideLösungsmittel

Versuchsvorschrift

250 g of florfenicol was suspended in 330 ml of acetic 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 yellow solution was obtained in a few minutes. Stirring was continued for another 3 hours. After 3 hrs, the reaction mixture was poured into 1000 g of ice and stirring continued to arrive at a suspension of product. Solid present was filtered and resuspended in 500 ml of water, and then stirred for 10 min to remove residual acetic acid. The solid product was filtered using a Buckner funnel under vacuum and then recrystallized in ethanol. The recrystallized product was washed with hexane and dried to obtain around 260 g of solid florfenicol acetate.

Aufarbeitung

  1. customequipped with a over-head stirrer and a drying tube
  2. customA clear yellow solution was obtained in a few minutes
  3. stirringStirring
  4. waitAfter 3 hrs
  5. stirringstirring
  6. additionto arrive at a suspension of product
  7. filtrationSolid present was filtered
  8. stirringstirred for 10 min
  9. customto remove residual acetic acid
  10. filtrationThe solid product was filtered
  11. customrecrystallized in ethanol
  12. washThe recrystallized product was washed with hexane
  13. customdried

Quellen und Nachweise

ORD-Eintrag
ord-332703855af345a3b21cad011de7268e
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786167B2

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