Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Pyridoxamine, dihydrochloride | HCID 10664 | — |
| Edukt | Menadione sodium bisulfite (USP:INN) | HCID 23677974 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | Menadione | HCID 4055 | — |
Reaktionsschritte
A solution containing 2.0 grams of pyridoxamine dihydrochloride, purity 98%, (0.00813 moles), in 10 ml of water, at room temperature, was added dropwise during 5 minutes, to a stirred solution of 5.2 grams of menadione sodium bisulfite, purity 95%, (0.01496 moles), in 13 ml of water. After a few minutes of stirring at a temperature of 25° C., a white crystalline precipitate formed. The product was filtered, washed with a few milliliters of ice cold water, then dried in vacuum at 40°-45° C. until constant weight was achieved. The recovered dry product was a white crystalline powder weighing 5.05 grams. The assay gave a combined menadione content equal to 48.5%, with a yield (based on MSB) equal to 95% and a purity of 95.3%. The so obtained compound melted, with decomposition, at 171°-173° C. The product was moderately soluble in water (1.3 g/100 ml of water).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04808602 |
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| Quelldatensatz | uspto-grants-1989_02 |
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| ORD ID | ord-6a9fce84b9a94e0ea22e028637e667f8 |
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| Quellennotiz | uspto-grants-1989_02 |
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