関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 15-Crown-5 | HCID 36336 | — |
| 反応物 | (3-Chloropropyl)cyclohexane | HCID 70762 | — |
| 反応物 | sodium 3-(1-triphenylmethyl-1H-imidazol-4-yl)propanolate | HCID 23682245 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3-Cyclohexylpropyl 3-(1H-imidazol-4-yl)propyl ether | HCID 178420894 | — |
反応手順
5 mmol of sodium 3-[1-(triphenylmethyl)imidazol-4-yl]propoxide in 10 ml of toluene containing 0.5 mmol of 15-Crown-5 and 5 mmol of (3-chloropropyl)cyclohexane are mixed and the mixture is stirred for 24 h at 75° C. The suspension is concentrated under vacuum, the product obtained is dissolved in diethyl ether, the solution is filtered and the residue washed with petroleum ether (40°-60° C.). The filtrate obtained is concentrated and maintained for 1 h at the boiling point in a 2N aqueous/alcohol (ethanol/water) hydrochloric acid solution. The ethanol is removed under a low vacuum and the precipitate is filtered under vacuum. The solution is basified, extracted with dichloromethane and the organic phase is concentrated. The title compound obtained is recrystallized in the hydrogenmaleate form from ethanol/diethyl ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05559113 |
|---|
| 出典データセット | uspto-grants-1996_09 |
|---|
| ORD ID | ord-00b6922018944aca9cf64b1932ec59e1 |
|---|
| 出典メモ | uspto-grants-1996_09 |
|---|