化工社化工社化学信息打印报告 · 仅供科研参考
丙酮 → 克拉维酸钾
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 丙酮 | HCID 180 | — |
| 反应物 | 氟化锂 | HCID 224478 | — |
| 反应物 | 氟化钾 | HCID 522689 | — |
| 反应物 | 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 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 产物 | 克拉维酸钾 | HCID 23665591 | — |
反应步骤
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).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US04255332 |
| 来源数据集 | uspto-grants-1981_03 |
| ORD ID | ord-00469e0c5c164e47a7ad2220299dd984 |
| 来源说明 | uspto-grants-1981_03 |