Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-[4-(4-Fluorophenyl)-1,3-thiazol-2-yl]-N-pyrazin-2-ylpiperazine-1-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1-[4-(4-Fluorophenyl)-2-thiazolyl]piperazine | HCID 8027201 | — |
| 반응물 | 2,2,2-Trichloroethyl pyrazin-2-ylcarbamate | HCID 68777403 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 4-[4-(4-Fluorophenyl)-1,3-thiazol-2-yl]-N-pyrazin-2-ylpiperazine-1-carboxamide | HCID 68779098 | 34.1% |
반응 단계
A mixture if 2,2,2-trichloroethyl pyrazin-2-ylcarbamate (226 mg, 0.835 mmol), 4-[4-(4-fluorophenyl)-1,3-thiazol-2-yl]piperazine (200 mg, 0.760 mmol) and diisopropylethylamine (0.265 ml, 1.52 mmol) in dimethylsulfoxide (2.5 ml) was stirred at 70° C. for 3 days. Water was poured into the reaction solution, and the mixture was extracted with ethyl acetate. The extract was wash washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified silica gel column chromatography (ethyl acetate) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give the desired product (99.7 mg, 34.0%) as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07851473B2 |
| 출처 데이터셋 | uspto-grants-2010_12 |
| ORD ID | ord-996151c7ada64869bae11e6fd38fd5fa |
| 출처 메모 | uspto-grants-2010_12 |