Hydrochloric Acid → HCID 178511756、化合物

HRID 261713ノート

反応式

HRID 261713 の反応式
[Na].[SH:2][C:3]1[NH:7][N:6]=[N:5][CH:4]=1.[OH-].[Na+].[NH2:10][C@@H:11]1[C:39](=[O:40])[N:13]2[C:14]([C:36]([OH:38])=[O:37])=[C:15]([CH2:18]OC(=O)C3C=CC=CC=3C(=O)NC(OCC)=O)[CH2:16][S:17][C@H:12]12.Cl>O.CO>[NH2:10][C@@H:11]1[C:39](=[O:40])[N:13]2[C:14]([C:36]([OH:38])=[O:37])=[C:15]([CH2:18][S:2][C:3]3[NH:7][N:6]=[N:5][CH:4]=3)[CH2:16][S:17][C@H:12]12

参加物

8

反応物 5

HCID 313Hydrochloric Acid2 回HCID 14798Sodium HydroxideHCID 5360545SodiumHCID 705826067beta-amino-3-[2-(N-carboethoxycarbamoyl)benzoyloxy]methyl-3-cephem-4-carboxylic acidHCID 178527741HCID 178527741、化合物

生成物 1

HCID 178511756HCID 178511756、化合物収率 61.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

in water (2 ml) containing sodium salt of 5-mercapto-1H-1,2,3-triazole (120 mg) and sodium hydroxide (40 mg) is dissolved under ice cooling 7β-amino-3-[2-(N-carboethoxycarbamoyl)benzoyloxy]methyl-3-cephem-4-carboxylic acid (450 mg) and to the mixture is added diluted hydrochloric acid to adjust its pH to 5.5 under stirring, followed by further stirring for one hour at 60° C. To the solution, is added methanol (5 ml) and the mixture is allowed to cool to the room temperature. The cooled mixture is adjusted its pH to 3.9 by adding diluted hydrochloric acid under stirring and the resultant mixture is further stirred for one hour under ice-cooling. The precipitate is collected by filtration and washed with water and methanol in this order and then dried over phosphorus pentoxide. The procedure provides 7β-amino-3-(1H-1,2,3-triazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid (193 mg).

後処理

  1. dissolutionis dissolved under ice
  2. stirringby further stirring for one hour at 60° C
  3. stirringunder stirring
  4. temperaturecooling
  5. filtrationThe precipitate is collected by filtration
  6. washwashed with water and methanol in this order
  7. dry with materialdried over phosphorus pentoxide

出典と根拠

ORDレコード
ord-9aa8b46edf954ed49f2cb643c5798b44
出典データセット
uspto-grants-1979_08
特許番号
US04166178

反応ノート

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