참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2,2,2-Trichloroethyl pyridazin-3-ylcarbamate | HCID 68576698 | — |
| 반응물 | 1-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine | HCID 68776289 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 4-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]-N-pyridazin-3-ylpiperazine-1-carboxamide | HCID 11625525 | 35.3% |
반응 단계
A mixture of 2,2,2-trichloroethyl pyridazin-3-ylcarbamate (212 mg, 0.782 mmol), 1-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine (200 mg, 0.711 mmol) and diisopropylethylamine (0.248 ml, 1.42 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 70° C. for 3 days. Water was poured to the reaction mixture, 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 tetrahydrofuran to give 101 mg (35.2%) of the desired product as a solid. mp 215-216° C.
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-18035578c6604d61b3539557b06c52bd |
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| 출처 메모 | uspto-grants-2010_12 |
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