Acetone → Potassium Clavulanate

HRID 127157

Reaktionsgleichung

Reaktionsgleichung von HRID 127157
[Li+].[CH2:2]1[C:5](=[O:6])[N:4]2[C@@H:7]([C:13]([O-:15])=[O:14])/[C:8](/[O:12][C@H:3]12)=[CH:9]/[CH2:10][OH:11].[F-].[K+:17].[F-].[Li+].CC(C)=O>O>[CH2:2]1[C:5](=[O:6])[N:4]2[C@@H:7]([C:13]([O-:15])=[O:14])/[C:8](/[O:12][C@H:3]12)=[CH:9]/[CH2:10][OH:11].[K+:17]

Komponenten

6

Edukt 4

HCID 180AcetoneHCID 224478Lithium fluorideHCID 522689Potassium FluorideHCID 237146474-Oxa-1-azabicyclo[3.2.0]heptane-2-carboxylic acid, 3-(2-hydroxyethylidene)-7-oxo-, lithium salt (1:1), (2R,3Z,5R)-

Produkt 1

HCID 23665591Potassium Clavulanate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Lithium clavulanate (5.15 g, estimated purity 95% pfa; 0.025 moles) was dissolved in water (45 mls) and cooled in an ice bath. Potassium fluoride solution (2.82 g KF.2H2O, 1.2 eq in 7 ml water) was added over 15 mins. Lithium fluoride started to separate out after less than 1 ml had been added. Isopropanol (32 mls) was added over 1/2 hr and the mixture made up to 600 ml with acetone over 8 hr. The mixture was stirred with celite (2 gm) and filtered to give a clear, colourless solution. This was added with rapid stirring to acetone (1400 mls) over 1 hr and the white solid filtered off, washing with acetone (3×500 ml) and dried on a fluid bed dryer to yield potassium clavulanate (4.8 g, 82.9% pfa, 81% recovery).

Aufarbeitung

  1. temperaturecooled in an ice bath
  2. customto separate out after less than 1 ml
  3. additionhad been added
  4. additionIsopropanol (32 mls) was added over 1/2 hr
  5. filtrationfiltered
  6. customto give a clear, colourless solution
  7. additionThis was added
  8. filtrationthe white solid filtered off
  9. washwashing with acetone (3×500 ml)
  10. customdried on a fluid bed dryer

Quellen und Nachweise

ORD-Eintrag
ord-00469e0c5c164e47a7ad2220299dd984
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255332

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