Hydrochloric Acid → HCID 5362051, 화합물

HRID 542912

반응식

HRID 542912 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].Cl>>[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 2

HCID 313Hydrochloric AcidHCID 5481173Ceftazidime

생성물 1

HCID 5362051HCID 5362051, 화합물

반응 조건

온도
5 °C

실험 절차

Another 131 ml aliquot of the ceftazidime solution prepared as described above was adjusted to and maintained at 5° C. and the pH adjusted to 3.5 with 15.2 ml of 1.83M hydrochloric acid. The stirred solution was seeded with ceftazidime pentahydrate crystals and crystallization began. After one hour, the pH of the crystal slurry was readjusted from 4.55 to 3.50 with an additional 2.90 ml of 1.83M hydrochloric acid. The slurry was stirred for three more hours and then filtered. The crystals were washed with 150 ml of chilled water and 100 ml of chilled acetone and air dried. There were obtained 19.3 g of ceftazidime pentahydrate which assayed as follows: HPLC potency, 83.2% (as is); polymer (stressed), 0.82%; related substances, 1.04%; Karl Fischer, 13.9%.

후처리

  1. customThe stirred solution was seeded with ceftazidime pentahydrate crystals and crystallization
  2. filtrationfiltered
  3. washThe crystals were washed with 150 ml of chilled water and 100 ml of chilled acetone and air
  4. customdried

출처 및 근거

ORD 기록
ord-146a7f2c4d814ccda17c039b626a7072
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659813

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