참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 1-(1-Benzylpiperidin-4-yl)-2-(2-fluorophenyl)ethanol | HCID 22248173 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-(1-Benzylpiperidin-4-yl)-2-(2-fluorophenyl)ethanone | HCID 22247993 | 73% |
반응 단계
After dissolving 7.5 ml of oxalyl chloride in 130 ml of dichloromethane, the solution was cooled to −78° C. and a solution of 6.1 ml of dimethylsulfoxide in dichloromethane (20 ml) was added dropwise while stirring. After stirring for 20 minutes, a solution of 13.4 g of 1-(1-benzylpiperidin-4-yl)-2-(2-fluorophenyl)ethanol in dichloromethane (40 ml) was added dropwise. After stirring for 30 minutes, 24 ml of triethylamine was added and the temperature was raised to room temperature. Water was added to the reaction solution, the organic layer was washed with water and saturated brine in that order and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by NH silica gel column chromatography (solvent: n-hexane/ethyl acetate) to obtain the title compound (9.64 g, 73% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07915274B2 |
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| 출처 데이터셋 | uspto-grants-2011_03 |
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| ORD ID | ord-722ea4779f1247ca9b73bbff3e9331fa |
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| 출처 메모 | uspto-grants-2011_03 |
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