Reaktion #73573

ord-0d412acdfa6949519a58c094e4bf455b

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 78.9%

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 15 L of acetone was added to the resulting solid
  4. 4
    FiltrationInsoluble material was filtered
  5. 5
    Einengenthe filtrate was concentrated under reduced pressure

Vorschrift

2 kg (1 equivalent) of metformin hydrochloride and 483 g (1 equivalent) of sodium hydroxide were stirred in 10 L of methanol for 2 hours at room temperature, and then remaining solid was filtered and the filtrate was concentrated under reduced pressure. Then 15 L of acetone was added to the resulting solid and stirred. Insoluble material was filtered, and the filtrate was concentrated under reduced pressure to obtain 1,230 g of metformin free base. The metformin free base was dissolved in 33 L of acetone, 2.8 L (4 equivalents) of acetic acid was added, and then the mixture was stirred for 2 hours at room temperature. The resulting crystal was filtered, and re-crystallized in water and acetone to obtain 1,089 g of metformin acetate (yield: 47.7%).

Quelle

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