참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3,3-Diphenylpropyl methanesulfonate | HCID 22238292 | — |
| 반응물 | 3-Methylpyrrolidin-3-ol hydrochloride | HCID 53346559 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 1-(3,3-Diphenylpropyl)-3-methylpyrrolidin-3-ol | HCID 89961746 | 57% |
반응 단계
To a 10 L reaction flask were added 3-methylpyrrolidin-3-ol hydrochloride (616 g, 4.48 mol), anhydrous potassium carbonate (1186 g, 8.6 mol) and acetonitrile (5 L). To the resulting mixture was slowly added a solution of 3,3-diphenylpropyl methanesulfonate (1000 g, 3.45 mol) in acetonitrile dropwisely at 85° C. The reaction was conducted for 12 hours. After the completion of reaction monitored by TLC, the reaction solution was evaporated under reduced pressure to remove acetonitrile. A mixed solution of dichloromethane and water was added for extraction. The organic phase was dried over anhydrous sodium sulfate, and evaporated to remove the solvent to produce a crude product, which was purified by column chromatography (silica gel column, eluted with petroleum ether: ethyl acetate=50:1 (volumetric ratio)) to produce 1-(3,3-diphenylpropyl)-3-methylpyrrolidin-3-ol (580 g) in a yield of 57%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09198902B2 |
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| 출처 데이터셋 | uspto-grants-2015_12 |
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| ORD ID | ord-46599b8306124f56911108474c6cb3f3 |
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| 출처 메모 | uspto-grants-2015_12 |
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