反应详情

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).

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