Methanol → Potassium Clavulanate

Lithium clavulanate (5.6 gm, estimated purity 88.8% pfa 0.025 M) was dissolved in water (45 mls) and the resulting pale-red-brown solution was cooled in an ice bath. Tripotassium orthophosphate (10.1 mls of 1 M solution, 1.2 equivalents) was added in one lot and methanol (18 mls) added over 1/2 hr with a small quantity of lithium phosphate (ca. 1 mg) for seeding. As lithium phosphate separated out the pH dropped from 8.7 to about 7.5. Acetone was added over 3/4 hr to 800 mls. The material that separated out was quite orange-brown at this point and the supernatant a very pale yellow. Celite (2 g) filtration gave a clear solution which was added to acetone (1750 mls) with vigorous stirring over 1 hr. The white solid was filtered off leaving a very pale yellow filtrate. Washing with acetone (3×50 ml) and fluid bed drying gave potassium clavulanate (4.1 g, 84% pfa, 69% recovery).

1. temperaturethe resulting pale-red-brown solution was cooled in an ice bath
2. customAs lithium phosphate separated out the pH
3. additiondropped from 8.7 to about 7.5
4. additionAcetone was added over 3/4 hr to 800 mls
5. customThe material that separated out
6. filtrationCelite (2 g) filtration
7. customgave a clear solution which
8. filtrationThe white solid was filtered off
9. customleaving a very pale yellow filtrate
10. washWashing with acetone (3×50 ml) and fluid bed
11. customdrying

ORDレコード

ord-0741b8df57ba42faa0d52d03226d448a

出典データセット

uspto-grants-1981_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04255332