関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Amantadine | HCID 2130 | — |
| 反応物 | 1,4-Dioxane-2,6-dione | HCID 78232 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | [2-(1-Adamantylamino)-2-oxoethoxy]acetic Acid | HCID 7357748 | — |
反応手順
In a similar operation, a solution of 11.56 g (0.100 mole) of diglycolic anhydride in 1 liter of dichloromethane was added with stirring to a solution of 15.11 grams (0.100 mole) of 1-adamantanamine in 700 milliliters of dichloromethane during about 24 minutes at about 15° to 25° C., whereupon a reaction took place with the formation of heterogeneous milky white mixture. The mixture was stirred for 3.67 hours at temperatures of about 23°-25° C. to complete the reaction with the formation of the desired product in the reaction mixture. The mixture was then concentrated on a rotary evaporator to recover 32.7 grams of a white solid which after recrystallization from 1:1 isopropanol-water mixture yielded the desired [2-(1-adamantylamino)-2-oxoethoxy]acetic acid as white plates, m.p. 181°-183° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04306063 |
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| 出典データセット | uspto-grants-1981_12 |
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| ORD ID | ord-d8ffa236f9a7497e83290e487bd6c0de |
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| 出典メモ | uspto-grants-1981_12 |
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