Hydrochloric Acid → 7-Amino-3-azidomethyl-3-cephem-4-carboxylic acid

HRID 1722558ノート

反応式

HRID 1722558 の反応式
C(O[CH2:5][C:6]1[CH2:7][S:8][C@@H:9]2[CH:16]([NH2:17])[C:15](=[O:18])[N:10]2[C:11]=1[C:12]([OH:14])=[O:13])(=O)C.[N-:19]=[N+:20]=[N-:21].[Na+].C(=O)(O)[O-].[Na+].Cl>P([O-])([O-])([O-])=O>[NH2:17][CH:16]1[C:15](=[O:18])[N:10]2[C:11]([C:12]([OH:14])=[O:13])=[C:6]([CH2:5][N:19]=[N+:20]=[N-:21])[CH2:7][S:8][C@H:9]12

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 33557Sodium AzideHCID 516892Sodium Bicarbonate2 回HCID 113463103-Acetoxymethyl-7-amino-3cephem-4-carboxylic acid

生成物 1

HCID 128022197-Amino-3-azidomethyl-3-cephem-4-carboxylic acid収率 40%

試薬・触媒・溶媒 1

HCID 1061Phosphate溶媒

実験手順

To a stirred suspension of 3-acetoxymethyl-7-aminoceph-3-em-4-carboxylic acid (45.3 g.) in a phosphate buffer (pH 6.4; 700 ml.) was added sodium azide (10.8 g.), then in small portions sodium bicarbonate (14 g.). The stirred mixture was then immersed in a 60° bath for 6 hours, the pH being maintained at 6.4 by addition of 2N aqueous HCl or 5% w/v aqueous sodium bicarbonate solutions. After cooling the pH of the mixture was adjusted to 3-3.5 with 2N aqueous HCl. The resulting precipitate was separated, washed with water and acetone then dried over P2O5 to give 7-amino-3-azidomethylceph-3-em-4-carboxylic acid (40%).

後処理

  1. customwas then immersed in a 60°
  2. customfor 6 hours
  3. temperatureAfter cooling the pH of the mixture
  4. customThe resulting precipitate was separated
  5. washwashed with water and acetone
  6. dry with materialthen dried over P2O5

出典と根拠

ORDレコード
ord-a9308b05b0784700a648c78d76cf77b7
出典データセット
uspto-grants-1989_08
特許番号
US04855420

反応ノート

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