氟化锂 → 克拉维酸钾

HRID 127160

反应方程式

HRID 127160 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].[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]

参与物

5

反应物 3

HCID 224478氟化锂HCID 522689氟化钾HCID 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克拉维酸钾收率 60.7%

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 (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).

后处理

  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

来源与证据

ORD记录
ord-5a61272768264719a1a123a8b1ca1acc
来源数据集
uspto-grants-1981_03
专利号
US04255332

关联笔记

加载中…