참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | 15-Crown-5 | HCID 36336 | — |
| 반응물 | (3-Chloropropyl)cyclohexane | HCID 70762 | — |
| 반응물 | sodium 3-(1-triphenylmethyl-1H-imidazol-4-yl)propanolate | HCID 23682245 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 3-Cyclohexylpropyl 3-(1H-imidazol-4-yl)propyl ether | HCID 178420894 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05559113 |
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| 출처 데이터셋 | uspto-grants-1996_09 |
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| ORD ID | ord-00b6922018944aca9cf64b1932ec59e1 |
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| 출처 메모 | uspto-grants-1996_09 |
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