Sodium Bicarbonate → HCID 88770327, Verbindung

HRID 127098Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 127098
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

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 23681836Potassium 1-methyl-1H-tetrazole-5-thiolateHCID 88769766HCID 88769766, Verbindung

Produkt 1

HCID 88770327HCID 88770327, VerbindungAusbeute 49,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1061PhosphateLösungsmittel

Versuchsvorschrift

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.).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-a1f95acbfa2e4c048eda6d4b10bb73c4
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04254260

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