참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 4-[4-(3-Fluorophenyl)-1,3-thiazol-2-yl]piperidine | HCID 62541778 | — |
| 반응물 | 2,2,2-Trichloroethyl pyridazin-3-ylcarbamate | HCID 68576698 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 4-[4-(3-fluorophenyl)-1,3-thiazol-2-yl]-N-pyridazin-3-ylpiperidine-1-carboxamide | HCID 68778005 | 43.8% |
반응 단계
A mixture of 2,2,2-trichloroethyl pyridazin-3-ylcarbamate (250 mg, 0.922 mmol), 4-[4-(3-fluorophenyl)-1,3-thiazol-2-yl]piperidine (220 mg, 0.839 mmol) and diisopropylethylamine (0.292 ml, 1.68 mmol) in dimethylsulfoxide (2.8 ml) was stirred at 70° C. for 6 hours. Water was poured into the reaction solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate) and recrystallized from a mixed solvent of hexane and ethyl acetate to give the desired product (141 mg, 43.7%) as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07851473B2 |
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| 출처 데이터셋 | uspto-grants-2010_12 |
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| ORD ID | ord-9a677cc7118f4e66b3e78751cd43ef57 |
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| 출처 메모 | uspto-grants-2010_12 |
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