関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Urea | HCID 1176 | — |
| 反応物 | 1-Bromo-3,5-dimethyladamantane | HCID 98317 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 生成物 | Memantine | HCID 4054 | — |
反応手順
To 100 g of 1-bromo-3,5-dimethyl adamantane and 86 g of urea, adding 80 ml of 80 wt % formic acid, heating to 80° C. and holding for 3 hours. Cooling to the room temperature and adding 95 ml of concentrated hydrochloric acid to hydrolyze at 80° C. for about 1 hour. Adjusting with 30% sodium hydroxide to a pH of 12, extracting with toluene twice, combining the organic layers and washing with water. Concentrating under reduced pressure to yield a limpid yellow solution as the 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 ethanol to yield 61.0 g of pure Memantine Hydrochloride. The yield of product is 68.8% (GC 99.5%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07355080B2 |
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| 出典データセット | uspto-grants-2008_04 |
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| ORD ID | ord-af27ba54084b434ead7b5cf9d1b0792c |
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| 出典メモ | uspto-grants-2008_04 |
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