Ceftazidime → HCID 5362051, 화합물

HRID 542911

반응식

HRID 542911 반응식
[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]

참가 물질

3

반응물 1

HCID 5481173Ceftazidime

생성물 1

HCID 5362051HCID 5362051, 화합물

시약·촉매·용매 1

HCID 284Formic Acid용매

반응 조건

온도
5 °C

실험 절차

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%.

후처리

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

출처 및 근거

ORD 기록
ord-0dabe3162f394c3c9bfcf7d27151ad10
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659813

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