Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Lithium fluoride | HCID 224478 | — |
| Edukt | Potassium Fluoride | HCID 522689 | — |
| Edukt | 4-Oxa-1-azabicyclo[3.2.0]heptane-2-carboxylic acid, 3-(2-hydroxyethylidene)-7-oxo-, lithium salt (1:1), (2R,3Z,5R)- | HCID 23714647 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | Potassium Clavulanate | HCID 23665591 | 60,7% |
Reaktionsschritte
Lithium clavulanate (7.15 g, estimated purity 68% pfa 0.025 moles) was stirred in water (45 mls) and cooled in ice. Potassium fluoride solution (3.5 g KF.2H2O in 9 mls solution; 1.5 equivalents) was added slowly to the cloudy brown solution and lithium fluoride separated out as a fairly gummy deposit. The mixture was made up to 100 ml with acetone over 3/4hr and then up to 800 mls with acetone over 1/2 hr. The solid which had separated now was dark brown and was removed by filtration through celite (4 gm). The almost colourless filtrate was added to acetone (1750 ml) over 1 hr with rapid agitation, then filtered and washed with acetone (3×50 ml) and fluid bed dried to give a fine granular just off-white solid potassium clavulanate (3.6 g, 83.1% pfa, 62% recovery).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04255332 |
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| Quelldatensatz | uspto-grants-1981_03 |
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| ORD ID | ord-5a61272768264719a1a123a8b1ca1acc |
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| Quellennotiz | uspto-grants-1981_03 |
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