四氧化硫 → 克拉维酸钾

HRID 3626

反应方程式

HRID 3626 反应方程式
C(OCC)(=O)C.[CH2:7]1[C:10](=[O:11])[N:9]2[C@@H:12]([C:18]([OH:20])=[O:19])/[C:13](/[O:17][C@H:8]12)=[CH:14]/[CH2:15][OH:16].S(=O)(=O)(O)O.C(C(CCCC)C([O-])=O)C.[K+:36]>C(C(C)=O)C(C)C>[CH2:7]1[C:10](=[O:11])[N:9]2[C@@H:12]([C:18]([O-:20])=[O:19])/[C:13](/[O:17][C@H:8]12)=[CH:14]/[CH2:15][OH:16].[K+:36]

参与物

6

反应物 4

HCID 1118四氧化硫HCID 8857乙酸乙酯HCID 5280980克拉维酸HCID 23669619Potassium 2-ethylhexanoate

产物 1

HCID 23665591克拉维酸钾收率 73%

试剂、催化剂与溶剂 1

HCID 79094-甲基-2-戊酮溶剂2 次

反应条件

温度
5 °C

实验过程

100 ml of the solvent mixture of ethyl acetate and methyl isobutyl ketone (4:1) already cooled to 5° C. was added to 100 ml of aqueous solution containing clavulanic acid (12 mg/ml). While agitating the mixture, 50% sulfuric acid was slowly added in order to control pH at 1.5. After extracting the said mixture, the extracts are separated. The remaining aqueous solution was further extracted with 100 ml of the solvent mixture three times. Anhydrous magnesium sulfate (10 g) and activated carbon(10 g) were added to the combined extract, and the resultant mixture was agitated at 5° C. for 30 minutes. The mixture was suction-filtered through a filter, and the remaining material was washed with 50 ml of methyl isobutyl ketone. A solution of potassium 2-ethylhexanoate (1.5 equivalent) dissolved in methyl isobutyl ketone was slowly added to the said extract, and the mixture was agitated at 5° C. for 2 hours. The crystalline product was filtered and slurried with acetone at the same temperature for 2 hours. The crystalline was dried in a vacuum desiccator (30° C.) for about 5 hours to obtain 1.07 g of potassium clavulanate (yield: 73%).

后处理

  1. additionwas slowly added in order
  2. extractionAfter extracting the said mixture
  3. customthe extracts are separated
  4. extractionThe remaining aqueous solution was further extracted with 100 ml of the solvent mixture three times
  5. additionAnhydrous magnesium sulfate (10 g) and activated carbon(10 g) were added to the
  6. extractioncombined extract
  7. filtrationThe mixture was suction-filtered through a filter
  8. washthe remaining material was washed with 50 ml of methyl isobutyl ketone
  9. additionwas slowly added to the
  10. extractionsaid extract
  11. stirringthe mixture was agitated at 5° C. for 2 hours
  12. filtrationThe crystalline product was filtered
  13. waitslurried with acetone at the same temperature for 2 hours
  14. customThe crystalline was dried in a vacuum desiccator (30° C.) for about 5 hours

来源与证据

ORD记录
ord-aa33d2dcc235487b9f952619afa7f8ab
来源数据集
uspto-grants-1998_03
专利号
US05734048

关联笔记

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