Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 5-Bromo-6-fluoro-3-[(E)-2-(4-fluorophenyl)vinyl]-1-trityl-1H-indazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Fluorostyrene | HCID 67883 | — |
| 반응물 | 2-(Di-tert-butylphosphino)biphenyl | HCID 2734215 | — |
| 반응물 | 5-Bromo-6-fluoro-3-iodo-1-trityl-1H-indazole | HCID 68930723 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-Bromo-6-fluoro-3-[(E)-2-(4-fluorophenyl)vinyl]-1-trityl-1H-indazole | HCID 68930056 | 74.1% |
반응 단계
A solution of 3.0 g of 5-bromo-6-fluoro-3-iodo-1-trityl-1H-indazole, 628 mg of 4-fluorostyrene, 115 mg of palladium acetate, 307 mg of 2-(di-ter-butylphosphino)biphenyl and 3.60 mL of triethylamine in N,N-dimethylformamide was stirred at 70° C. for a day. After diluting with ethyl acetate, washing successively with aqueous ammonium chloride and saturated brine, and drying over anhydrous magnesium sulfate, the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:100), to afford 2.2 g of the title compound as colorless crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07429609B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-d6adc56acf8a425a97c316cf88ec27c7 |
| 출처 메모 | uspto-grants-2008_09 |