Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Urea | HCID 1176 | — |
| Edukt | 1-Bromo-3,5-dimethyladamantane | HCID 98317 | — |
| Lösungsmittel | Formic Acid | HCID 284 | — |
| Produkt | Memantine | HCID 4054 | — |
Reaktionsschritte
To 100 g of 1-bromo-3,5-dimethyl adamantane and 86 g of urea, adding 72 ml of 94 wt % formic acid, heating to 120° C. and holding for 2 hours. Cooling to the room temperature and adding 385 ml of 10% hydrochloric acid to hydrolyze at 100° C. for about 1 hour. Adjusting with 30% sodium hydroxide solution to a pH of 12, extracting with butyl acetate twice, combining the organic layers and washing with water. Concentrating under reduced pressure to yield a limpid yellow solution as 1-amino-3,5-dimethyl adamantane crude. To the crude, adding 150 ml of ethanol and concentrated hydrochloric acid, heating to dissolve and crystallizing to yield white solid. Drying the solid and re-crystallizing with water to yield 60.4 g of pure Memantine Hydrochloride. The yield is 68.1% (GC 99.1%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07355080B2 |
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| Quelldatensatz | uspto-grants-2008_04 |
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| ORD ID | ord-a459468c271b451aa9b5c056101e5890 |
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| Quellennotiz | uspto-grants-2008_04 |
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