関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Amantadine Hydrochloride | HCID 64150 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 3-Amino-1-adamantanol | HCID 658645 | — |
反応手順
To a mixture of 150 ml of concentrated sulfuric acid and 15 ml of concentrated nitric acid, cooled to 10° C. is added 10 g (0.053 moles) of 1-adamantanamine hydrochloride over 5 minutes. This mixture is stirred in an ice bath for 4 hours. The reaction is then poured over ice and the pH adjusted to pH 10 using 50% NaOH. The product is extracted into chloroform which is dried over MgSO4 and then evaporated to dryness. The residue is recrystallized from ethyl acetate to give 3-hydroxytricyclo[3.3.1.13,7 ]decan-1-amine (m.p. 260°-264° C.) which is used directly in step B.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05596020 |
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| 出典データセット | uspto-grants-1997_01 |
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| ORD ID | ord-6e7885fc1cc547e48924216fe5c21fea |
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| 出典メモ | uspto-grants-1997_01 |
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