Methane → Cefdinir monohydrate

HRID 898083

Reaktionsgleichung

Reaktionsgleichung von HRID 898083
[CH2:1]=[CH:2][C:3]1[CH2:23][S:22][C@@H:6]2[C@H:7]([NH:10][C:11](/[C:13](/[C:16]3[N:20]=[C:19]([NH2:21])[S:18][CH:17]=3)=[N:14]\[OH:15])=[O:12])[C:8](=[O:9])[N:5]2[C:4]=1[C:24]([OH:26])=[O:25].C(=O)(O)[O-:28].[Na+].C>O>[CH2:1]=[CH:2][C:3]1[CH2:23][S:22][C@@H:6]2[C@H:7]([NH:10][C:11](/[C:13](/[C:16]3[N:20]=[C:19]([NH2:21])[S:18][CH:17]=3)=[N:14]\[OH:15])=[O:12])[C:8](=[O:9])[N:5]2[C:4]=1[C:24]([OH:26])=[O:25].[OH2:28]

Komponenten

5

Edukt 3

HCID 297MethaneHCID 516892Sodium BicarbonateHCID 6915944Cefdinir

Produkt 1

HCID 11993766Cefdinir monohydrate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

The monohydrate was prepared as follows: Cefdinir (20.0 g) was added to water (200 ml) and the mixture was adjusted to pH 6.0 with saturated sodium bicarbonate aqueous solution. The resultant solution was subjected to a column chromatography on activated charcoal and eluted with 20% aqueous acetone. Fractions were combined and then concentrated to 200 ml. This solution was adjusted to pH 2.2 at 15° C. with 10% hydrochloric acid and stirred at 0° C. for 30 minutes. The resultant crystals were collected by filtration, washed with water and dried to give crystals of Cefdinir monohydrate. The present inventors investigated physicochemical properties for Cefdinir monohydrate and crystal form A. The results are described below.

Aufarbeitung

  1. washeluted with 20% aqueous acetone
  2. concentrationconcentrated to 200 ml
  3. customwas adjusted to pH 2.2 at 15° C. with 10% hydrochloric acid
  4. filtrationThe resultant crystals were collected by filtration
  5. washwashed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-52f6304a211841e38c522993a859a60c
Quelldatensatz
uspto-grants-2008_04
Patentnummer
US07351419B2

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