Sodium Bicarbonate → HCID 88770327、化合物

HRID 127098ノート

反応式

HRID 127098 の反応式
C(O[CH2:5][C:6]1[CH2:7][S:8][C@@H:9]2[CH:16]([NH:17][C:18](=[O:26])[CH2:19][C:20]3[S:24][C:23]([NH2:25])=[N:22][CH:21]=3)[C:15](=[O:27])[N:10]2[C:11]=1[C:12]([OH:14])=[O:13])(=O)C.[CH3:28][N:29]1[C:33]([S-:34])=[N:32][N:31]=[N:30]1.[K+].C(=O)(O)[O-].[Na+]>P([O-])([O-])([O-])=O>[CH3:28][N:29]1[C:33]([S:34][CH2:5][C:6]2[CH2:7][S:8][C@@H:9]3[CH:16]([NH:17][C:18](=[O:26])[CH2:19][C:20]4[S:24][C:23]([NH2:25])=[N:22][CH:21]=4)[C:15](=[O:27])[N:10]3[C:11]=2[C:12]([OH:14])=[O:13])=[N:32][N:31]=[N:30]1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 23681836Potassium 1-methyl-1H-tetrazole-5-thiolateHCID 88769766HCID 88769766、化合物

生成物 1

HCID 88770327HCID 88770327、化合物収率 49.4%

試薬・触媒・溶媒 1

HCID 1061Phosphate溶媒

実験手順

A solution of 3-acetoxymethyl-7-(2-aminothiazol-5-yl)acetamido-3-cephem-4-carboxylic acid (2 g.) and potassium 1-methyl-1H-tetrazole-5-thiolate (0.7 g.) in pH 6.4 phosphate buffer (50 ml.) was stirred for 4 hours with continuous introduction of nitrogen gas while the reaction mixture was kept to pH 6.4 to 7 with sodium bicarbonate. After the reaction, the reaction mixture was cooled and then filtered. The filtrate was adjusted to pH 2.5 with diluted hydrochloric acid under ice-cooling, and the precipitates were collected by filtration and then purified similarly as that of Example 6 to give light brown powder of 3-(1-methyl-1H-tetrazol-5-yl)thiomethyl-7-(2-aminothiazol-5-yl)acetamido-3-cephem-4-carboxylic acid (1.05 g.).

後処理

  1. customAfter the reaction
  2. temperaturethe reaction mixture was cooled
  3. filtrationfiltered
  4. temperaturecooling
  5. filtrationthe precipitates were collected by filtration
  6. custompurified similarly as that of Example 6

出典と根拠

ORDレコード
ord-a1f95acbfa2e4c048eda6d4b10bb73c4
出典データセット
uspto-grants-1981_03
特許番号
US04254260

反応ノート

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