Ethanol → Potassium Clavulanate

HRID 127156

Reaktionsgleichung

Reaktionsgleichung von HRID 127156
[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].P([O-])([O-])([O-])=O.[K+:21].[K+].[K+].C(O)C.P([O-])([O-])([O-])=O.[Li+].[Li+].[Li+]>O.CC(C)=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+:21]

Komponenten

7

Edukt 4

HCID 702EthanolHCID 62657Potassium Phosphate, TribasicHCID 165867Lithium phosphateHCID 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 ClavulanateAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittelHCID 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. Tripotassium orthophosphate (10.1 mls of 1 M solution; 1.2 equivalents) was added in one lot. Ethanol (32 mls) was added slowly over 1/2 hour by which time lithium phosphate had precipitated out and the pH had fallen from 8.3 to 7.3. The mixture was then made up to 800 mls with acetone over 3/4 hr. Celite (2 gm) was added and then the mixture was filtered to give a clear, colourless filtrate. This was added with rapid stirring to acetone (1750 mls) over 1 hr and the white solid was filtered off, washed with acetone (3×50 mls) 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. customhad precipitated out
  3. waitThe mixture was then made up to 800 mls with acetone over 3/4 hr
  4. additionCelite (2 gm) was added
  5. filtrationthe mixture was filtered
  6. customto give a clear, colourless filtrate
  7. additionThis was added
  8. filtrationthe white solid was filtered off
  9. washwashed with acetone (3×50 mls)
  10. customdried on a fluid bed dryer

Quellen und Nachweise

ORD-Eintrag
ord-93c4962afafc47268f71341e3f652412
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04255332

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