참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,2-Diphenylethyl methanesulfonate | HCID 11747820 | — |
| 반응물 | 3-Methylpyrrolidin-3-ol hydrochloride | HCID 53346559 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 1-(2,2-Diphenylethyl)-3-methylpyrrolidin-3-ol | HCID 89961805 | 58.23% |
반응 단계
According to Example 15, 3-methylpyrrolidin-3-ol hydrochloride was synthesized. To a 500 mL reaction flask were added 3-methylpyrrolidin-3-ol hydrochloride (11.46 g, 83 mmol), anhydrous potassium carbonate (28.75 g, 208 mmol) and acetonitrile (220 mL). To the resulting mixture was slowly added a solution of 2,2-diphenylethyl methanesulfonate (23 g, 83 mmol) in acetonitrile dropwisely at 85° C. The reaction was conducted for 12 hours. After the completion of reaction monitored by TLC, the resulting mixture 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. The crude product was purified by column chromatography (silica gel column, eluted with petroleum ether:ethyl acetate=30:1 (volumetric ratio)) to produce 1-(2,2-diphenylethyl)-3-methylpyrrolidin-3-ol (13.6 g) in a yield of 58.23%.
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-e8ed6fa782a14dee921fc287f6951eb8 |
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| 출처 메모 | uspto-grants-2015_12 |
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