Acetic Acid → HCID 178476642, Verbindung

HRID 45296

Reaktionsgleichung

Reaktionsgleichung von HRID 45296
[CH3:1][N:2]([C:4]([NH:6][C:7]([NH2:9])=[NH:8])=[NH:5])[CH3:3].[C:10]([OH:13])(=[O:12])[CH3:11]>CC(C)=O>[CH3:1][N:2]([C:4]([NH:6][C:7]([NH2:9])=[NH:8])=[NH:5])[CH3:3].[C:10]([O-:13])(=[O:12])[CH3:11]

Komponenten

4

Edukt 2

HCID 176Acetic AcidHCID 178484382HCID 178484382, Verbindung

Produkt 1

HCID 178476642HCID 178476642, VerbindungAusbeute 47,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel2×

Versuchsvorschrift

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%).

Aufarbeitung

  1. filtrationThe resulting crystal was filtered
  2. customre-crystallized in water

Quellen und Nachweise

ORD-Eintrag
ord-1d4ddea1485044f8bf175bad0b24f4a1
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08541474B2

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