Reaktion #64271

ord-03cfd62b56564b7aaa9029b192fcff22

Reaktionsgleichung

COC(=O)c1ccc(O)cc1
Methyl paraben
CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)[C@H](N)c3ccccc3)[C@H]2SC1.O
cephalexin monohydrate
COC(=O)c1ccc(O)cc1
methyl paraben
CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)[C@H](N)c3ccccc3)[C@H]2SC1
cephalexin
[F-].[K+]
KF
→
COC(=O)c1ccc(O)cc1.O
Methyl Paraben·H2O

Edukte

COC(=O)c1ccc(O)cc1
Methyl paraben
CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)[C@H](N)c3ccccc3)[C@H]2SC1.O
cephalexin monohydrate
COC(=O)c1ccc(O)cc1
methyl paraben
—
( 67.1 )
CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)[C@H](N)c3ccccc3)[C@H]2SC1
cephalexin
[F-].[K+]
KF
—
( 3.5 )

Reagenzien

Keine

Lösungsmittel

O
water
O
water

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto result in a suspension
  2. 2
    Filtrationthe crystals were collected by filtration
  3. 3
    Waschenwashed with water
  4. 4
    Sonstigeto give 1.06 g (2.0 mmol) of cocrystals

Vorschrift

Methyl paraben (375 mg, 2.5 mmol) in 150 ml of water was added to cephalexin monohydrate (2.4 g, 6.6 mmol) to result in a suspension. After 5 days at 5° C., the crystals were collected by filtration and washed with water to give 1.06 g (2.0 mmol) of cocrystals. mp 168°-169° C. Anal. calcd for C24H25N3O7S·H2O: C, 55.70; H, 5.26; N, 8.12. Found: C, 55.65; H, 5.28; N, 8.13. HPLC assay (calcd), found: (67.1), 67.1% cephalexin, (29.4), 28.7% methyl paraben. KF (Calcd) , found: (3.5) , 4.0% water.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05412094uspto-grants-1995_05