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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Lithium fluoride → Potassium Clavulanate

HRID 127160
ノート
印刷プレビュー

反応式

HRID 127160 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].[F-].[K+:17].[F-].[Li+]>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+:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 224478Lithium fluorideHCID 522689Potassium FluorideHCID 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収率 60.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Lithium clavulanate (7.15 g, estimated purity 68% pfa 0.025 moles) was stirred in water (45 mls) and cooled in ice. Potassium fluoride solution (3.5 g KF.2H2O in 9 mls solution; 1.5 equivalents) was added slowly to the cloudy brown solution and lithium fluoride separated out as a fairly gummy deposit. The mixture was made up to 100 ml with acetone over 3/4hr and then up to 800 mls with acetone over 1/2 hr. The solid which had separated now was dark brown and was removed by filtration through celite (4 gm). The almost colourless filtrate was added to acetone (1750 ml) over 1 hr with rapid agitation, then filtered and washed with acetone (3×50 ml) and fluid bed dried to give a fine granular just off-white solid potassium clavulanate (3.6 g, 83.1% pfa, 62% recovery).

後処理

  1. temperaturecooled in ice
  2. customseparated out as a fairly gummy deposit
  3. waitThe mixture was made up to 100 ml with acetone over 3/4hr
  4. customThe solid which had separated now was dark brown
  5. customwas removed by filtration through celite (4 gm)
  6. additionThe almost colourless filtrate was added to acetone (1750 ml) over 1 hr with rapid agitation
  7. filtrationfiltered
  8. washwashed with acetone (3×50 ml) and fluid bed
  9. customdried

出典と根拠

ORDレコード
ord-5a61272768264719a1a123a8b1ca1acc
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04255332

反応ノート

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