Isopropanol → Potassium Clavulanate

HRID 127154

반응식

HRID 127154 반응식
[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].C(O)(C)C.P([O-])([O-])([O-])=O.[K+:25].[K+].[K+].P([O-])([O-])([O-])=O.[Li+].[Li+].[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+:25]

참가 물질

6

반응물 4

HCID 3776IsopropanolHCID 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)-

생성물 1

HCID 23665591Potassium Clavulanate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Lithium clavulanate (21.9 g, estimated purity 67% as pure free acid, 3/40 mole) was stirred in distilled water (135 mls) and isopropanol added (108 mls) with stirring and cooling in an ice bath. The supernatant liquid was decanted off the gummy precipitate (6.0 gm) and a solution (37.8 mls 1.5 eq) of 1 M potassium orthophosphate added slowly with about 20 mg lithium phosphate for seeding. As lithium phosphate separated the pH changed from 8.2 to 7.1 ending up at 7.65 on total addition. The mixture was made up to 500 mls with acetone and filtered and the clear yellow filtrate was divided into 3 equal portions. Portion 1 was made up to 600 mls with acetone, filtered via celite (2 gm) and added to 2.4 liters acetone slowly with stirring. The white solid was filtered off, washed with acetone and fluid bed dried to give potassium clavulanate (4.94 g, 82.1% pfa, 83% recovery). Portion 2 was made up to 800 mls, filtered as above and added to 2.2 l acetone. The solid was filtered off and dried to give potassium clavulanate (4.88 g, 81.9% pfa, 82% recovery). Portion 3 was made up to 1000 mls, filtered as above and added to 2 l acetone. The solid was filtered off and dried to give potassium clavulanate (4.84 g, 82.3 pfa, 82% recovery).

후처리

  1. temperaturecooling in an ice bath
  2. customThe supernatant liquid was decanted off the gummy precipitate (6.0 gm)
  3. customAs lithium phosphate separated the pH
  4. additionchanged from 8.2 to 7.1 ending up at 7.65 on total addition
  5. filtrationfiltered
  6. filtrationfiltered via celite (2 gm)
  7. additionadded to 2.4 liters acetone slowly
  8. stirringwith stirring
  9. filtrationThe white solid was filtered off
  10. washwashed with acetone and fluid bed
  11. customdried

출처 및 근거

ORD 기록
ord-535806152dcb4222b990ec60d35e69f0
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255332

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