Hydrochloric Acid → HCID 5362051、化合物

HRID 542912

反応式

HRID 542912 の反応式
[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]

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 5481173Ceftazidime

生成物 1

HCID 5362051HCID 5362051、化合物

反応条件

温度
5 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-146a7f2c4d814ccda17c039b626a7072
出典データセット
uspto-grants-1987_04
特許番号
US04659813

関連ノート

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