참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Fluorostyrene | HCID 67883 | — |
| 반응물 | 2-(Di-tert-butylphosphino)biphenyl | HCID 2734215 | — |
| 반응물 | 3-bromo-6-fluoro-5-nitro-1-trityl-1H-indazole | HCID 68928300 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 6-Fluoro-3-[(E)-2-(4-fluorophenyl)-vinyl]-5-nitro-1-trityl-1H-indazole | HCID 68928492 | 46.8% |
반응 단계
To a solution of 600 mg of 3-bromo-6-fluoro-5-nitro-1-trityl-1H-indazole in 6 mL of N,N-dimethylformamide were successively added 292 mg of 4-fluorostyrene, 71 mg of 2-(di-tert-butylphosphino)biphenyl, 27 mg of palladium acetate (II) and 0.85 mL of triethylamine, and stirred at 80° C. for 6.5 hours. The solvent was evaporated, and the resulting residue was dissolved in 25 mL of ethyl acetate. The organic layer was successively washed with water (twice) and saturated brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated. The obtained crude crystal was recrystallized from ethyl acetate-diisopropylether, to afford 304 mg of the title compound as bright yellow crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07429609B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-3c4fee8c4bba47369bf067c0e1d01924 |
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| 출처 메모 | uspto-grants-2008_09 |
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