참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Piperidin-3-ylmethanol | HCID 107308 | — |
| 반응물 | 1-(p-Chlorophenyl)cyclobutanecarboxylic acid | HCID 602761 | — |
| 반응물 | PyBroP | HCID 2733179 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-[1-(4-Chloro-phenyl)-cyclobutanecarbonyl]-piperidin-3-ylmethyl alcohol | HCID 21902035 | 43.4% |
반응 단계
To a solution of 3-piperidinemethanol (5.0 g, 43.4 mmol), 1-(4-chlorophenyl)-1-cyclobutanecarboxylic acid (9.14 g, 43.4 mmol), and diisopropylethylamine (11.22 g, 86.8 mmol) in dichloromethane (100 mL) at 0° C. was added PyBroP® (22.26 g, 47.8 mmol). The reaction was stirred at 0° C. for 1 h and then at room temperature for 4 h. The reaction mixture was washed successively with water, 1 N HCl, water, sat. sodium bicarbonate solution, and water (100 mL each). The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated by rotary evaporation. The residue was purified by chromatography on silica gel, eluting with dichloromethane/methanol (96:4) to give 5.8 g of the amide 1 as a thick gum.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07511141B2 |
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| 출처 데이터셋 | uspto-grants-2009_03 |
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| ORD ID | ord-e6dc98f870d84313bb53e8114f279824 |
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| 출처 메모 | uspto-grants-2009_03 |
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