反応式
[CH3:1][N:2]([C:4]([N:6]=[C:7]([NH2:9])[NH2:8])=[NH:5])[CH3:3].Cl.[OH-].[Na+]>CO>[CH3:1][N:2]([C:4]([NH:6][C:7]([NH2:9])=[NH:8])=[NH:5])[CH3:3]参加物
実験手順
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%).
後処理
- filtrationwas filtered
- concentrationthe filtrate was concentrated under reduced pressure
- additionThen 15 L of acetone was added to the resulting solid
- filtrationInsoluble material was filtered
- concentrationthe filtrate was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-0d412acdfa6949519a58c094e4bf455b
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541474B2
関連ノート
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