참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | (Bis(2-methoxyethyl)amino)sulfur trifluoride | HCID 2734690 | — |
| 반응물 | tert-Butyl 4-hydroxy-[1,4'-bipiperidine]-1'-carboxylate | HCID 9835508 | — |
| 생성물 | HCID 53419027 | HCID 53419027 | 60% |
반응 단계
Deoxo-Fluor® was added to a solution of 1,1-dimethylethyl 4-hydroxy-1,4′-bipiperidine-1′-carboxylate (0.500 g, 1.76 mmol) dropwise at −78° C. The mixture was maintained at −78° C. for 30 min before it was warmed to room temperature and stirred for 2 h. The mixture was washed with saturated aqueous sodium bicarbonate. The organic phase was dried over Na2SO4, filtered, and concentrated in vacuo. The crude material was purified via column chromatography (1:200 methanol/methylene chloride) to afford 1,1-dimethylethyl 4-fluoro-1,4′-bipiperidine-1′-carboxylate (0.300 g, 60% yield) as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08658636B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-75d10dc72c0c4ec2945bb9e80a22e50c |
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| 출처 메모 | uspto-grants-2014_02 |
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