Reaktion #1174425

ord-d6e5cb56217c42d09ba0764af2c6af55

Reaktionsgleichung

CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)[C@H](N)c3ccccc3)[C@H]2SC1
cephalexin
→
CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)[C@H](N)c3ccccc3)[C@H]2SC1.O
cephalexin monohydrate

Edukte

CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)[C@H](N)c3ccccc3)[C@H]2SC1
cephalexin

Reagenzien

Keine

Lösungsmittel

CC(C)O
IPA

Reaktionsbedingungen

Temperatur
1°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONthe pH was slowly lowered to 7.7 by acid addition [step (e)]
  2. 2
    Sonstigeafter crystallization
  3. 3
    workup.ADDITIONthe pH was lowered in 0.1 pH unit increments by acid addition to pH 7.0 [step (f)]

Vorschrift

IPA (16 liters) was added to the aqueous phase and the pH was slowly lowered to 7.7 by acid addition [step (e)]. The system was seeded with cephalexin and, after crystallization began, the pH was lowered in 0.1 pH unit increments by acid addition to pH 7.0 [step (f)], and finally to pH 5.0 [step (h)]. The crystal slurry was chilled to 1° C. for 1 hour [step (g)], then centrifuged to obtain a cephalexin monohydrate product [step (h)].

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05034522uspto-grants-1991_07