関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Metformin Hydrochloride | HCID 14219 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178484382 | HCID 178484382 | 78.9% |
反応手順
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%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08541474B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-0d412acdfa6949519a58c094e4bf455b |
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| 出典メモ | uspto-grants-2013_09 |
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