丙酮 → 克拉维酸钾

HRID 127155

反应方程式

HRID 127155 反应方程式
[Li+].[CH2:2]1[C:5](=[O:6])[N:4]2[C@@H:7]([C:13]([O-:15])=[O:14])/[C:8](/[O:12][C@H:3]12)=[CH:9]/[CH2:10][OH:11].P([O-])([O-])([O-])=O.[K+:21].[K+].[K+].P([O-])([O-])([O-])=O.[Li+].[Li+].[Li+].CC(C)=O>O>[CH2:2]1[C:5](=[O:6])[N:4]2[C@@H:7]([C:13]([O-:15])=[O:14])/[C:8](/[O:12][C@H:3]12)=[CH:9]/[CH2:10][OH:11].[K+:21]

参与物

6

反应物 4

HCID 180丙酮HCID 62657POTASSIUM DIPHOSPHATEHCID 165867Lithium phosphateHCID 237146474-Oxa-1-azabicyclo[3.2.0]heptane-2-carboxylic acid, 3-(2-hydroxyethylidene)-7-oxo-, lithium salt (1:1), (2R,3Z,5R)-

产物 1

HCID 23665591克拉维酸钾

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

Lithium clavulanate (5.15 g, estimated purity 95% pfa, 0.025 moles) was dissolved in 45 mls water and cooled in an ice bath. Tripotassium orthophosphate (10.1 mls of 1 M solution; 1.2 equivs) was added in one lot. The solution was seeded with lithium orthophosphate (1 mg) and acetone (20 ml) added over 1/2 hr. By this time a large quantity of lithium phosphate had separated out and the pH dropped from 8.3 to 7.4. The solution was made up to 100 ml with acetone over 20 minutes and was then made up to 800 mls with acetone over a further 10 minutes. The mixture was stirred with celite (2 gms) and filtered. The clear filtrate was added to acetone (1750 mls) over 1 hr. The white solid was filtered off and washed with acetone (3×50 ml) (being careful not to pull dry on the filter), and dried on a fluid bed dryer to yield potassium clavulanate (5 g, 83.0% pfa, 85% recovery).

后处理

  1. temperaturecooled in an ice bath
  2. additionadded over 1/2 hr
  3. customBy this time a large quantity of lithium phosphate had separated out
  4. additionthe pH dropped from 8.3 to 7.4
  5. waitwas then made up to 800 mls with acetone over a further 10 minutes
  6. filtrationfiltered
  7. additionThe clear filtrate was added to acetone (1750 mls) over 1 hr
  8. filtrationThe white solid was filtered off
  9. washwashed with acetone (3×50 ml) (
  10. customto pull dry on the
  11. filtrationfilter), and
  12. customdried on a fluid bed dryer

来源与证据

ORD记录
ord-0d9965bd1fc5453b8f1b3df09164fb12
来源数据集
uspto-grants-1981_03
专利号
US04255332

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