Acetone → Potassium Clavulanate

HRID 127155

反応式

HRID 127155 の反応式
[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]

参加物

6

反応物 4

HCID 180AcetoneHCID 62657Potassium Phosphate, TribasicHCID 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)-

生成物 1

HCID 23665591Potassium Clavulanate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0d9965bd1fc5453b8f1b3df09164fb12
出典データセット
uspto-grants-1981_03
特許番号
US04255332

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