Reaktion #73581

ord-803f6ad3e1704048a534d2078654b5ca

Reaktionsgleichung

CN(C)C(=N)N=C(N)N.Cl
metformin hydrochloride
[Na+].[OH-]
sodium hydroxide
CN(C)C(=N)NC(=N)N
metformin
Ausbeute 76.9%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationwas filtered
  2. 2
    Einengenthe filtrate was concentrated under reduced pressure
  3. 3
    workup.ADDITIONThen 300 Ml of acetone was added to the resulting solid
  4. 4
    FiltrationInsoluble material was filtered
  5. 5
    Einengenthe filtrate was concentrated under reduced pressure

Vorschrift

20.00 g (1 equivalent) of metformin hydrochloride and 4.84 g (1 equivalent) of sodium hydroxide were stirred in 200 Ml of ethanol for 2 hours at room temperature, and then remaining solid was filtered and the filtrate was concentrated under reduced pressure. Then 300 Ml of acetone was added to the resulting solid and stirred. Insoluble material was filtered, and the filtrate was concentrated under reduced pressure to obtain 12.0 g of metformin free base. 500 Ml of acetone and 10 Ml (1.45 equivalents) of glacial acetic acid were added to the metformin free base, and then the mixture was stirred. The resulting crystal was filtered and washed with acetone, and then dried at 60° C. to obtain 13.6 g of metformin acetate (yield: 59.5%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541474B2uspto-grants-2013_09