Ceftazidime → HCID 5362051, Verbindung

HRID 542911

Reaktionsgleichung

[CH3:1][C:2]([O:7]/[N:8]=[C:9](\[C:16]([NH:18][C@@H:19]1[C:22](=[O:23])[N:21]2[C:24]([C:35]([O-:37])=[O:36])=[C:25]([CH2:28][N+:29]3[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH2:26][S:27][C@H:20]12)=[O:17])/[C:10]1[N:14]=[C:13]([NH2:15])[S:12][CH:11]=1)([C:4]([OH:6])=[O:5])[CH3:3]>C(O)=O>[CH3:3][C:2]([O:7]/[N:8]=[C:9](/[C:16]([NH:18][C@@H:19]1[C:22](=[O:23])[N:21]2[C:24]([C:35]([O-:37])=[O:36])=[C:25]([CH2:28][N+:29]3[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH2:26][S:27][C@H:20]12)=[O:17])\[C:10]1[N:14]=[C:13]([NH2:15])[S:12][CH:11]=1)([C:4]([OH:6])=[O:5])[CH3:1].[OH2:5].[OH2:5].[OH2:5].[OH2:5].[OH2:5]

Komponenten

Reaktionsbedingungen

Temperatur: 5 °C

Versuchsvorschrift

A second 128 ml aliquot of the ceftazidime solution prepared as described above was cooled and maintained at 5° C., while the pH was adjusted from 5.8 to 3.6 with 10.5 ml of 5.9M formic acid. The stirred solution was seeded with ceftazidime pentahydrate crystals and crystallization commenced. After 5 hours the crystals were harvested by filtration, washed with 150 ml of chilled water and 100 ml of chilled acetone and air dried to give 20.8 g of ceftazidime pentahydrate. The material assayed as follows: HPLC potency 84.4% (as is); polymer (stressed material) 0.66%; related substances, 1.07%; Karl Fischer 14.1%.

Aufarbeitung

temperatureabove was cooled
customThe stirred solution was seeded with ceftazidime pentahydrate crystals and crystallization
filtrationAfter 5 hours the crystals were harvested by filtration
washwashed with 150 ml of chilled water and 100 ml of chilled acetone and air
customdried

Quellen und Nachweise

ORD-Eintrag: ord-0dabe3162f394c3c9bfcf7d27151ad10
Quelldatensatz: uspto-grants-1987_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04659813

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