関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-(Tricyclo(3.3.1.1'3,7)dec-1-yl)ethanol | HCID 110810 | — |
| 反応物 | 1-Acetyl-2-n-butyl 5-acetoxymethyl imidazole | HCID 19793547 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Chloroform methanol | HCID 21584188 | — |
| 生成物 | 5-Acetoxymethyl-1-[2-(1-adamantyl)ethyl]2-n-butylimidazole | HCID 19936797 | — |
反応手順
A mixture of 2-(1-adamantyl)ethanol (10.7 g and diisopropylethylamine (11 ml) in methylene chloride (70 ml) was added to triflic anhydride (16.75 g) in methylene chloride (70 ml) at -78° C. under argon. After stirring the mixture at -78° C. for 45 minutes, 1-acetyl-2-n-butyl-5 -(acetoxymethyl)imidazole in methylene chloride (50 ml) was added and the mixture was allowed to stand at room temperature for 4 days, then concentrated and heated on a steam bath with 10% sodium hydroxide (250 ml), diluted with 300 ml of water, extracted with methylene chloride, dried, filtered and concentrated to give an oil. Chromatography (silica gel) in methanol-chloroform gives 5-acetoxymethyl-1-[2-(1-adamantyl)ethyl]-2-n-butylimidazole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05418250 |
|---|
| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-8fab5ecdfc72432688ab3105276996ac |
|---|
| 出典メモ | uspto-grants-1995_05 |
|---|
